CN106748784A - A kind of method that high-purity methyl acetate is extracted in the industrial production waste liquid from terephthalic acid (TPA) - Google Patents
A kind of method that high-purity methyl acetate is extracted in the industrial production waste liquid from terephthalic acid (TPA) Download PDFInfo
- Publication number
- CN106748784A CN106748784A CN201611079740.4A CN201611079740A CN106748784A CN 106748784 A CN106748784 A CN 106748784A CN 201611079740 A CN201611079740 A CN 201611079740A CN 106748784 A CN106748784 A CN 106748784A
- Authority
- CN
- China
- Prior art keywords
- methyl acetate
- purity
- rectifying
- extractant
- purity methyl
- 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
- 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
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of method of the present invention direct high-purity methyl acetate in being mainly to provide industrial production waste liquid from terephthalic acid (TPA).The waste liquid containing methyl acetate that will be produced in terephthalic acid (TPA) industrial production, the method being combined by lateral line discharging rectifying and extractive distillation with salt, high-purity methyl acetate conveniently and is inexpensively obtained, to overcome be difficult with single rectification method or extraction and the deficiency of high-purity methyl acetate is directly obtained by waste liquid, it is to avoid the shortcoming of complex process in current method of purification.After waste liquid is through treatment in the present invention, more than 99.6% methyl acetate is can obtain.The technical process is simple, and energy consumption is low, is easy to industrialization.
Description
Technical field
The invention belongs to chemical production technical field, and in particular to one kind is extracted from terephthalic acid (TPA) industrial production waste liquid
The method of high-purity methyl acetate.
Background technology
Methyl acetate as a kind of new basic chemical raw materials, with a series of fine qualities such as low boiling, strong dissolving
Power, it is nuisanceless the advantages of, purposes is extremely wide, and belongs to environment-friendly products, and market usage amount is just amplified year by year.
At present, thick methyl acetate (75%, 92%) is accepted by user extensively as a kind of low side solvent product.And it is high
Purity methyl acetate, because its stable performance, evaporation rate are fast, during allotment diluent, using all without drawing under any ratio
The phenomenon such as " burning glue " " turning white " is played, it uses field and usage amount progressively to expand, price and usage amount are considerably beyond thick tumer
Ester.
In the production process of terephthalic acid (TPA) industry, a large amount of waste liquids containing methyl acetate can be produced, because these are useless
Also vinegar is limited in liquid containing ten several impurity such as substantial amounts of methyl alcohol, water and a small amount of acetic acid, n-propyl acetate, dimethylbenzene
The application industrially of sour methyl esters.Many producers are in recovery process mainly by being hydrolyzed into acetic acid and methyl alcohol at present, and
Reuse or sale aborning after being purified respectively.Greatly, the requirement to equipment is also high, the acetic acid of generation for the energy consumption of this process
Lacked competitiveness compared with the acetic acid and methyl alcohol that carbonylation is directly produced are in price with methyl alcohol, and cause the huge energy and material
The waste of material.In addition, purity 90% or so methyl acetate waste liquid the market price at 2000 yuan/ton or so, and purity exists
The market price of more than 99.6% high-purity methyl acetate is then at 6000~8000 yuan/ton.Therefore, methyl acetate waste liquid is given birth to
Producing into the methyl acetate of high-purity has larger economic benefit.It is more impurity for this kind of waste liquid main bugbear, and acetic acid
Methyl esters can form azeotropic with first alcohol and water, and high-purity methyl acetate is hardly resulted in simple rectifying.Chen Jian et al. uses azeotropic
The method and extracting rectifying of distillation, adsorptive distillation, condensing reflux and desorption and regeneration, liquid phase adsorption, alternating temperature purging desorption and regeneration
Method high-purity methyl acetate can be extracted from waste liquid, but technical process is more complicated, is not suitable for heavy industrialization.
The content of the invention
Goal of the invention：For weak point of the prior art, can be from terephthalic acid (TPA) work the invention provides one kind
The method that more than 99.6% high-purity methyl acetate is directly extracted in the waste liquid of industry production.To be produced in terephthalic acid (TPA) industrial production
The raw waste liquid containing methyl acetate, the method being combined by lateral line discharging rectifying and extractive distillation with salt is conveniently cheap
High-purity methyl acetate is obtained, to overcome be difficult with single rectification method or extraction high-purity tumer be directly obtained by waste liquid
The deficiency of ester, it is to avoid the shortcoming of complex process in current method of purification.
Technical scheme：The invention provides a kind of method for extracting high-purity methyl acetate, comprise the following steps：
A, with the waste liquid in terephthalic acid (TPA) industrial production as raw material, carries out unilateral line rectifying, obtains light component, heavy constituent
And the component that boiling point is 56~58 DEG C；
B, rectifying is carried out by gained heavy constituent in step a, and rectifying obtains the steam rich in methyl acetate, reclaims, and delivers to step
Rapid a circulations；
C, extracting rectifying, the light component that extracting rectifying is obtained are carried out by the component that gained boiling point in step a is 56~58 DEG C
It is high-purity methyl acetate, restructuring is divided into saliferous mixed liquor；
D, rectifying is carried out by gained saliferous mixed liquor in step c, and gained restructuring is divided into extractant, and delivering to step c circulations makes
With；Gained light component carries out rectification under vacuum；
E, step d rectification under vacuum gained restructuring are divided into methyl alcohol；Gained light component is methyl acetate, the c circulations of feeding step.
Further, in described raw material containing methyl acetate, methyl alcohol, acetic acid, benzoic acid, n-propyl acetate, to methyl
Benzaldehyde, dimethylbenzene, water.Due to the presence of acetic acid and dimethylbenzene, respectively can be with water formation azeotropic mixture, and water and methyl acetate
Form azeotropic mixture so that the methyl acetate difficulty for isolating high-purity is very big.
Further, the reflux ratio of unilateral line rectifying is 10~20 described in step a, and it is 60~70 to control bottom temperature
℃.The vapor (steam) temperature of lateral line discharging rectifying side take-off is 56~58 DEG C, and the number of plates of extractive distillation column is 50~60, and side line goes out
Expect the feed entrance point of rectifying side take-off steam at the 25th~30 column plate.Lateral line discharging tower bottom of rectifying tower obtains high boiling heavy
Component, into methyl acetate recovery tower recycling use.
Further, in the extracting rectifying described in step c, the extractant for being used is sub- for the diformazan containing inorganic salts
One kind or its mixture in sulfone, repefral.The preferred sodium acid carbonate of described inorganic salts, magnesium chloride, potassium chloride.
The volume ratio of dimethyl sulfoxide and repefral is 1~5 in the extractant：1, the content of inorganic salts is accounted for
The 5~10% of extractant total amount.Extractant is 1~2 with the volume ratio of raw material:1.
Further, in the extracting rectifying described in step c, reflux ratio is 2~5, controls tower top temperature for 57~58 DEG C,
Bottom temperature is 62~65 DEG C.Extractive distillation column reclaim obtain saliferous mixed liquor, the saliferous mixed liquor through extractant regeneration tower at
Reason, methyl acetate cut and methanol fraction are obtained in tower top, and regenerating extracting agent is obtained in the bottom of towe of extractant regeneration tower.
Further, the reflux ratio of rectification under vacuum described in step d is 2~3, and tower reactor pressure is 0.1atm, controls tower reactor
Temperature is 30~32 DEG C.
Specifically, the method and step of direct high-purity methyl acetate is such as from terephthalic acid (TPA) industrial production waste liquid
Under：
Will contain methyl acetate Production of Terephthalic Acid waste liquid feeding lateral line discharging rectifying column, control bottom temperature be 60~
70 DEG C, reflux ratio is 10~20, and the lower boiling steam of overhead extraction, tower reactor is high boiling heavy constituent, and side take-off boiling point exists
56~58 DEG C of steam, the steam is directly sent to extractive distillation column extracting rectifying；The heavy constituent of tower reactor is returned into recovery tower rectifying
The steam rich in methyl acetate is received, feedstock circulation is delivered to and is used.
The number of plates of extractive distillation column be 50~60, the feed entrance point of raw material at the 25th~30 column plate, extractant feed
At the 4th~6 column plate.The tower top temperature of the extractive distillation column is 57~58 DEG C, and bottom temperature is 66~68 DEG C, and reflux ratio is
3~5, the extractant is 1 with the volume ratio of raw material:1.Improved as one kind of technical solution of the present invention, from extractive distillation column
Saliferous mixed liquor is obtained, the saliferous mixed liquor is processed through extractant regeneration tower, obtains methyl acetate cut in tower top and methyl alcohol evaporates
Point, obtain regenerating extracting agent in the bottom of towe of extractant regeneration tower.The methanol fraction is processed through vacuum rectification tower, obtains byproduct
Methyl alcohol.
More specifically, a preferred plan of the invention is the Production of Terephthalic Acid waste liquid feeding side line containing methyl acetate
Discharging rectifying column, controls bottom temperature for 63 DEG C, and reflux ratio is 15, the lower boiling steam of overhead extraction, and tower reactor is high boiling
Heavy constituent, steam of the side take-off boiling point at 56~58 DEG C, steam is directly sent to extractive distillation column extracting rectifying；The weight of tower reactor
Component enters recovery tower rectifying and reclaims the steam rich in methyl acetate, delivers to feedstock circulation and uses.
The number of plates of extractive distillation column is 55, and at the 26th column plate, extractant is in the 5th block of column plate for the feed entrance point of raw material
Place.The tower top temperature of the extractive distillation column is 57~58 DEG C, and bottom temperature is 66~68 DEG C, and reflux ratio is 5, the extractant
It is the repefral solution containing 8wt% sodium acid carbonates, extractant is 1 with the volume ratio of raw material:1.Gained acetic acid
Methyl esters purity is 99.68%.
Beneficial effect：The direct high-purity methyl acetate from terephthalic acid (TPA) industrial production waste liquid that the present invention is provided
Method, step is fairly simple compared with current technique, and energy consumption is low, and extractant can be recycled.Waste liquid warp containing methyl acetate
After this method separating treatment, more than 99.6% high-purity methyl acetate is can obtain, the rate of recovery is up to 98%.Technical process letter
Single, energy consumption is low, non-wastewater discharge, is adapted to industrialization.
Brief description of the drawings
Fig. 1 is process flow diagram of the invention
In figure：The mono- lateral line discharging rectifying columns of B1-, B2- recovery towers, B3- extractive distillation columns, B4- extractant regeneration towers, B5-
Vacuum rectification tower.
Specific embodiment：
The technological process reference picture 1 of high-purity methyl acetate, wherein FEED tables are directly extracted from terephthalic acid (TPA) by-product
Show Production of Terephthalic Acid waste liquid, D1 represents lower boiling steam, W1 represents high boiling heavy constituent, F represent boiling point 56~
58 DEG C of steam, D3 represents the component containing methyl acetate, and S represents saliferous extractant, and P represents high-purity methyl acetate, and R is represented
Saliferous mixed liquor, S1 represents regenerating extracting agent, and D represents the light components such as methyl alcohol, and M represents methyl alcohol, and E is represented and evaporated containing a small amount of methyl acetate
Point.
Specifically, the methyl acetate solution for using Yangtze petrochemical industry chemical plant P3 to provide is raw material, through gas chromatographic analysis, group
Turn into：Methyl acetate 0.9025, methyl alcohol 0.0378, water 0.02, other 0.0397, composition be mass content.Production procedure is：
Production of Terephthalic Acid waste liquid FEED containing methyl acetate is sent into lateral line discharging rectifying column B1, bottom temperature is controlled
It it is 60~80 DEG C, reflux ratio is 10~20, the lower boiling steam D1 of overhead extraction, tower reactor is high boiling heavy constituent W1, side line
Steam F of the extraction boiling point at 56~58 DEG C, the steam is directly sent to B3 extractive distillation column extracting rectifyings；The heavy constituent W1 of tower reactor enters
Enter recovery tower B2 rectifying and reclaim the steam rich in methyl acetate, tower reactor is heavy seeds, and tower top D3 is methyl acetate steam, delivers to original
Material FEED is recycled.The methyl acetate steam F and saliferous extractant S of side take-off enter extractive distillation column B3, and tower top is obtained
High-purity methyl acetate P, bottom is that saliferous mixed liquor R, R carry out de- ester, dealcoholysis, dehydration, B4 towers into extractant regeneration tower B4
Bottom obtains regenerating extracting agent S1, returns to extractive distillation column B3 and recycles；The methanol fraction D that tower top is obtained enters vacuum rectification tower
B5 treatment, B5 tower reactors can obtain byproduct methyl alcohol M, and recovered overhead residue cut E, remaining cut E return to extractive distillation column B3
Recycle.
Embodiment 1,90% or so methyl acetate raw material feeding B1 lateral line discharging rectifying columns, it is 63 to control bottom temperature
DEG C, reflux ratio is 15, steam of the side take-off boiling point at 56~58 DEG C, and the steam is directly sent into B3 extractive distillation columns extraction essence
Evaporate；Tower top is the light impurity in raw material, and the heavy constituent of tower reactor enters B2 recovery towers and reclaims the steam rich in methyl acetate, and tower reactor is obtained
Heavy seeds in raw material, tower top is the steam rich in methyl acetate, delivers to feedstock circulation and uses.The methyl acetate of side take-off
The steam F and saliferous extractant S for preparing is with volume 1:(wherein, extractant S is repefral, carbonic acid to 1 ratio
Hydrogen sodium accounts for the 8wt% of extractant gross mass) enter extractive distillation column, specific extraction rectification technique parameter is shown in Table 1, from tower top sampling
Up to 99.68wt%, the rate of recovery is 98.2% to the purity of the high-purity methyl acetate P that mouth is obtained, from containing that bottom sample tap is released
Salt mixed liquor R flows into extractant regeneration tower B4 treatment.
The process conditions of extractant regeneration tower B4 are shown in Table 1, and saliferous mixed liquor R takes off ester, dealcoholysis, takes off through extractant regeneration tower B4
Regenerating extracting agent S1 is obtained from bottom of towe after water, extractive distillation column B3 is returned and is recycled；The methanol fraction D that tower top is obtained is flowed into and subtracted
Pressure rectifying column B5.
Through vacuum rectification tower B5 treatment, the number of plates is 15~25 to methanol fraction D, 30~32 DEG C of bottom temperature, reflux ratio 2~
3, tower reactor can obtain byproduct methyl alcohol M of the purity in more than 99wt%, and recovered overhead residue cut E, remaining cut E return to extraction
Take rectifying column B3 recyclings.
The technological parameter of the separation process of table 1
Embodiment 2
Operation is substantially the same manner as Example 1, and difference is：Single lateral line discharging tower bottom of rectifying tower temperature is 70 DEG C, is returned
Stream is than being 15；Dimethyl sulfoxide and repefral volume ratio 2 in extractant S:1, the methyl acetate steam F of side take-off
It is 1 with the input material volume ratio of extractant S:The high-purity methyl acetate P's that the tower top sample tap of 2, extractive distillation column B3 is obtained is pure
It is 99.65% to spend, and methyl acetate recovery rate is 98.5%.
Embodiment 3
Operation is substantially the same manner as Example 1, and difference is that single lateral line discharging tower bottom of rectifying tower temperature is 60 DEG C, backflow
Than being 12；Dimethyl sulfoxide and repefral volume ratio 1 in extractant S:1, magnesium chloride accounts for extractant gross mass
7wt%.The purity of the high-purity methyl acetate P that the tower top sample tap of extractive distillation column B3 is obtained is 99.60%, and methyl acetate is returned
Yield is 97.5%.
Embodiment 4
Operation is substantially the same manner as Example 1, and difference is that the extractive distillation column number of plates is 50, and reflux ratio is 7；Extraction
The composition of agent S is：Dimethyl sulfoxide and repefral volume ratio 3:1, magnesium chloride, sodium acid carbonate respectively account for the total matter of extractant
The input material volume ratio of the 3wt% of amount, the methyl acetate steam F and extractant S of side take-off is 1:2.The tower of extractive distillation column B3
The purity of the high-purity methyl acetate P that top sample tap is obtained is 99.65%, and methyl acetate recovery rate is 98.5%.
Embodiment 5
Operation is substantially the same manner as Example 1, and difference is that single lateral line discharging tower bottom of rectifying tower temperature is 68 DEG C, backflow
Than being 15；The number of theoretical plate (N) of extractive distillation column B3 is 60, and methyl acetate steam F feed entrance points (NF) of side take-off is 30,
Extractant feed position (NS) is 5.The purity of the high-purity methyl acetate P that the tower top sample tap of extractive distillation column B3 is obtained is
99.67%, methyl acetate recovery rate is 97.5%.
Embodiment 6
Operation is substantially the same manner as Example 1, and difference is that single lateral line discharging tower bottom of rectifying tower temperature is 62 DEG C, backflow
Than being 20；The composition of extractant S is：The volume ratio of dimethyl sulfoxide and repefral is 4：1, potassium chloride accounts for extractant
The input material volume ratio of the 8wt% of gross mass, the methyl acetate steam F and extractant S of side take-off is 1:2.Extractive distillation column B3
The purity of high-purity methyl acetate P that obtains of tower top sample tap be 99.63%, methyl acetate recovery rate is 98.8%.
Embodiment 7
Operation is substantially the same manner as Example 1, and difference is：Single lateral line discharging tower bottom of rectifying tower temperature is 63 DEG C, is returned
Stream is than being 20；Extractant S is dimethyl sulfoxide, and the high-purity methyl acetate P's that the tower top sample tap of extractive distillation column B3 is obtained is pure
It is 99.62% to spend, and methyl acetate recovery rate is 98.5%.
Embodiment 8
Operation is substantially the same manner as Example 1, and difference is：The composition of extractant S is：Dimethyl sulfoxide and O-phthalic
Dimethyl phthalate volume ratio 5:1, potassium chloride accounts for the 8wt% of extractant gross mass, what the tower top sample tap of extractive distillation column B3 was obtained
The purity of high-purity methyl acetate P is 99.61%, and methyl acetate recovery rate is 98.2%.
Embodiment 9
Operation is substantially the same manner as Example 1, and difference is：Extractant and unilateral line rectifying discharging evaporate in extracting rectifying
The volume ratio divided is 2:The purity of the high-purity methyl acetate P that the tower top sample tap of 1, extractive distillation column B3 is obtained is 99.68%,
Methyl acetate recovery rate is 98%.
Embodiment 10
Operation is substantially the same manner as Example 1, and difference is：Extractant S is dimethyl sulfoxide, potassium chloride, magnesium chloride, carbon
Sour hydrogen sodium respectively accounts for the 2wt% of extractant gross mass, and the input material volume ratio of the methyl acetate steam F and extractant S of side take-off is
1:1.The purity of the high-purity methyl acetate P that the tower top sample tap of extractive distillation column B3 is obtained is 99.62%, methyl acetate recovery
Rate is 98.1%.
Embodiment 11
Operation is substantially the same manner as Example 1, and difference is：Single lateral line discharging tower bottom of rectifying tower temperature is 60 DEG C, is returned
Than being 15, extractant S is dimethyl sulfoxide to stream, and the high-purity methyl acetate P's that the tower top sample tap of extractive distillation column B3 is obtained is pure
It is 99.60% to spend, and methyl acetate recovery rate is 95.5%.
Comparative example 1
Operation is substantially the same manner as Example 1, and difference is that single lateral line discharging tower bottom of rectifying tower temperature is 58 DEG C, backflow
Than being 12；The composition of extractant S is：Dimethyl sulfoxide and repefral volume ratio 1:1, it is total that sodium acid carbonate accounts for extractant
The 2wt% of quality.The purity of the high-purity methyl acetate P that the tower top sample tap of extractive distillation column B3 is obtained is 99.30%, acetic acid
The methyl esters rate of recovery is 97%.
Comparative example 2
Operation is substantially the same manner as Example 1, and difference is that single lateral line discharging tower bottom of rectifying tower temperature is 70 DEG C, backflow
Than being 8；The composition of extractant S is：Dimethyl sulfoxide and repefral volume ratio 1:4, potassium chloride accounts for the total matter of extractant
The 5wt% of amount.The purity of the high-purity methyl acetate P that the tower top sample tap of extractive distillation column B3 is obtained is 99.28%, tumer
The ester rate of recovery is 96%.
The bottom temperature when unilateral line rectifying column is can be seen that at 63~68 DEG C from above-mentioned experiment, and reflux ratio is 15~20
When, side take-off methyl acetate best results；When the extractive distillation column number of plates is that 45~50, reflux ratio is that 4~5, extractant is
During repefral containing 8wt% sodium acid carbonates, extracting rectifying best results.
Claims (8)
1. it is a kind of extract high-purity methyl acetate method, it is characterised in that comprise the following steps：
A, with the waste liquid in terephthalic acid (TPA) industrial production as raw material, carries out unilateral line rectifying, obtains light component, heavy constituent and boiling
Point is 56~58 DEG C of component；
B, rectifying is carried out by gained heavy constituent in step a, and rectifying obtains the steam rich in methyl acetate, reclaims, and delivers to step a and follows
Ring；
C, extracting rectifying is carried out by the component that gained boiling point in step a is 56~58 DEG C, and the light component that extracting rectifying is obtained is height
Purity methyl acetate, restructuring is divided into saliferous mixed liquor；
D, rectifying is carried out by gained saliferous mixed liquor in step c, and gained restructuring is divided into extractant, delivers to step c recyclings；Institute
Obtaining light component carries out rectification under vacuum；
E, step d rectification under vacuum gained restructuring are divided into methyl alcohol；Gained light component is methyl acetate, the c circulations of feeding step.
2. the method for extracting high-purity methyl acetate as claimed in claim 1, it is characterised in that contain vinegar in described raw material
Sour methyl esters, methyl alcohol, acetic acid, n-propyl acetate, benzoic acid, p-tolyl aldehyde, dimethylbenzene, water.
3. the method for extracting high-purity methyl acetate as claimed in claim 1, it is characterised in that unilateral line essence described in step a
The reflux ratio for evaporating is 10~20, and it is 60~70 DEG C to control bottom temperature.
4. the method for extracting high-purity methyl acetate as claimed in claim 1, it is characterised in that the extraction essence described in step c
In evaporating, the extractant for being used is the dimethyl sulfoxide containing inorganic salts, one kind of repefral or its mixture, institute
The inorganic salts stated are the mixture of one or more arbitrary proportions in sodium acid carbonate, magnesium chloride, potassium chloride.
5. the method for extracting high-purity methyl acetate as claimed in claim 1, it is characterised in that diformazan is sub- in the extractant
Sulfone, the proportioning of repefral are 1~5：1.
6. the method for extracting high-purity methyl acetate as claimed in claim 1, it is characterised in that the extraction essence described in step c
In evaporating, extractant is 1~2 with the volume ratio of raw material:1.
7. the method for extracting high-purity methyl acetate as claimed in claim 1, it is characterised in that the extraction essence described in step c
In evaporating, reflux ratio is 2~5, and it is 57~58 DEG C to control tower top temperature, and bottom temperature is 62~65 DEG C.
8. the method for extracting high-purity methyl acetate as claimed in claim 1, it is characterised in that gained rectification under vacuum in step d
Reflux ratio be 2~3, tower reactor pressure is 0.1atm, control bottom temperature for 30~32 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611079740.4A CN106748784A (en) | 2016-11-29 | 2016-11-29 | A kind of method that high-purity methyl acetate is extracted in the industrial production waste liquid from terephthalic acid (TPA) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611079740.4A CN106748784A (en) | 2016-11-29 | 2016-11-29 | A kind of method that high-purity methyl acetate is extracted in the industrial production waste liquid from terephthalic acid (TPA) |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106748784A true CN106748784A (en) | 2017-05-31 |
Family
ID=58901241
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611079740.4A Pending CN106748784A (en) | 2016-11-29 | 2016-11-29 | A kind of method that high-purity methyl acetate is extracted in the industrial production waste liquid from terephthalic acid (TPA) |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106748784A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295557A (en) * | 2011-07-06 | 2011-12-28 | 福州大学 | Method for refining methyl acetate as by-product in PVA production |
| CN104418734A (en) * | 2013-08-22 | 2015-03-18 | 中国石油化工股份有限公司 | Method for directly extracting high purity methyl acetate from byproduct in terephthalic acid industrial production |
-
2016
- 2016-11-29 CN CN201611079740.4A patent/CN106748784A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295557A (en) * | 2011-07-06 | 2011-12-28 | 福州大学 | Method for refining methyl acetate as by-product in PVA production |
| CN104418734A (en) * | 2013-08-22 | 2015-03-18 | 中国石油化工股份有限公司 | Method for directly extracting high purity methyl acetate from byproduct in terephthalic acid industrial production |
Non-Patent Citations (2)
| Title |
|---|
| 孙井智等: "工业生产中醋酸甲酯回收技术的研究进展", 《河北化工》 * |
| 顾美娟等: "精对苯二甲酸装置副产醋酸甲酯的提纯研究", 《南通职业大学学报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107501152B (en) | A kind of separation method of tert-butyl hydroperoxide | |
| CN106220532B (en) | A kind of method of separation of extractive distillation acetonitrile and triethylamine | |
| JP7486847B2 (en) | Method for producing ethylene acetate | |
| CN110885283A (en) | Energy-saving process for separating ethyl acetate-ethanol by heat integration extraction rectification with side extraction | |
| CN110156590A (en) | A method of spirit of vinegar is recycled based on extraction/azeotropic distillation coupling technique | |
| CN107311878A (en) | A kind of device for reclaiming glycine waste liquid and the method for reclaiming glycine waste liquid | |
| JPS6261312B2 (en) | ||
| CN103772185B (en) | Device and method for removing moisture and heteroacids in acetic acid | |
| CN111170823B (en) | Method for simultaneously extracting phenol and naphthalene from tar | |
| CN105669445B (en) | The production technology of ethyl acetate | |
| CN108329204B (en) | Concentration method of formic acid aqueous solution containing hydrogen chloride | |
| WO2022237654A1 (en) | Method and system for refining acrylic acid | |
| CN106748784A (en) | A kind of method that high-purity methyl acetate is extracted in the industrial production waste liquid from terephthalic acid (TPA) | |
| CN109503360A (en) | A kind of technique for spirit of vinegar recycling | |
| CN216129524U (en) | Separation refining plant for preparing methyl acetate from industrial tail gas | |
| CN106380403B (en) | The method for efficiently separating dimethyl oxalate and dimethyl carbonate | |
| CN212347768U (en) | Device for synthesizing trioxymethylene by salt effect reaction rectification | |
| CN111499495B (en) | Method for separating and recovering non-acidic oxygen-containing organic matters from Fischer-Tropsch synthesis water | |
| CN115057761A (en) | Method for producing purified ethyl tert-butyl ether by reactive distillation coupled extraction distillation dividing wall tower technology | |
| CN115028523A (en) | Pressure-variable-heterogeneous azeotropic rectification separation method for butanone dehydration | |
| CN107459448A (en) | A kind of acetic acid is separated from water method | |
| CN107459449A (en) | A kind of acetic acid is separated from water method | |
| CN102863334B (en) | Method for preparing high purity methyl acetate by adding salt, extracting and rectifying | |
| CN102863333B (en) | Method for extracting high purity methyl acetate in methyl acetate-methanol-water mixed liquor | |
| CN104418734A (en) | Method for directly extracting high purity methyl acetate from byproduct in terephthalic acid industrial production |
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: 20170531 |