CN110423197A - A kind of device and method using low concentration ethylene glycol production glycol acetate - Google Patents
A kind of device and method using low concentration ethylene glycol production glycol acetate Download PDFInfo
- Publication number
- CN110423197A CN110423197A CN201910874100.XA CN201910874100A CN110423197A CN 110423197 A CN110423197 A CN 110423197A CN 201910874100 A CN201910874100 A CN 201910874100A CN 110423197 A CN110423197 A CN 110423197A
- Authority
- CN
- China
- Prior art keywords
- tower
- ethylene glycol
- acetic acid
- removing column
- feed inlet
- 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.)
- Granted
Links
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 title claims abstract description 411
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 title claims abstract description 63
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 title claims abstract description 55
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 243
- 230000003197 catalytic effect Effects 0.000 claims abstract description 79
- 238000004821 distillation Methods 0.000 claims abstract description 66
- 239000002994 raw material Substances 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 239000002699 waste material Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000470 constituent Substances 0.000 claims abstract description 6
- 238000010992 reflux Methods 0.000 claims description 75
- 239000003054 catalyst Substances 0.000 claims description 53
- 239000000463 material Substances 0.000 claims description 44
- 239000007795 chemical reaction product Substances 0.000 claims description 30
- 239000012535 impurity Substances 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 14
- 230000032050 esterification Effects 0.000 claims description 13
- 238000005886 esterification reaction Methods 0.000 claims description 13
- 238000000926 separation method Methods 0.000 claims description 10
- 239000011973 solid acid Substances 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- BZYAZRQBOJRREG-UHFFFAOYSA-N acetic acid;ethane-1,2-diol Chemical compound CC(O)=O.CC(O)=O.OCCO BZYAZRQBOJRREG-UHFFFAOYSA-N 0.000 claims description 5
- 125000003827 glycol group Chemical group 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 3
- 229920005862 polyol Polymers 0.000 claims 1
- 150000003077 polyols Chemical class 0.000 claims 1
- HXDLWJWIAHWIKI-UHFFFAOYSA-N 2-hydroxyethyl acetate Chemical compound CC(=O)OCCO HXDLWJWIAHWIKI-UHFFFAOYSA-N 0.000 abstract description 4
- 239000011347 resin Substances 0.000 description 10
- 229920005989 resin Polymers 0.000 description 10
- 230000008901 benefit Effects 0.000 description 9
- -1 glycol ester Chemical class 0.000 description 9
- JTXMVXSTHSMVQF-UHFFFAOYSA-N 2-acetyloxyethyl acetate Chemical compound CC(=O)OCCOC(C)=O JTXMVXSTHSMVQF-UHFFFAOYSA-N 0.000 description 6
- 239000007787 solid Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- 239000003377 acid catalyst Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 150000002168 ethanoic acid esters Chemical class 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 229940083957 1,2-butanediol Drugs 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- BMRWNKZVCUKKSR-UHFFFAOYSA-N butane-1,2-diol Chemical compound CCC(O)CO BMRWNKZVCUKKSR-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000000449 nitro group Chemical class [O-][N+](*)=O 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000002895 organic esters Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000007592 spray painting technique Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of device and method using low concentration ethylene glycol production glycol acetate, and including sequentially connected preheater, fixed bed reactors, catalytic distillation tower, weight-removing column, lightness-removing column, treating column: the ethylene glycol and acetic acid of low concentration are reacted in fixed bed reactors;Primary product, which enters in catalytic distillation tower, to be continued catalytic distillation reaction and is separated, and the heavy constituent of tower bottom, which enters in weight-removing column, to be separated;The product of the tower top of weight-removing column is sent into lightness-removing column and is separated;The product of the tower bottom of lightness-removing column is sent into treating column and is separated, and the tower top for the treatment of column obtains product glycol acetate.The waste material that the present invention is generated using in ethylene glycol production process is turned waste into wealth as raw material, and glycol concentration is not less than 20%, concentration >=99.0% of obtained product glycol acetate, ethylene glycol acetate concentration≤1%, water≤0.1%, acetic acid≤0.2%.
Description
Technical field
The present invention relates to a kind of device and method for producing glycol acetate, and in particular to a kind of to utilize low concentration second
The device and method of glycol production glycol acetate produce high concentration second using low concentration ethylene glycol further to a kind of
The device and method of glycol diacetate.
Background technique
Glycol acetate is also known as ethylene acetate, diacetate glycol ester, is colourless liquid, boiling point 190.2
DEG C, it is efficient, safe and non-toxic environment-friendly type organic solvent.It is widely used in pharmaceuticals industry, foundry resin organic ester curing agent, is also made
For the fine solvent of various organic resins especially nitrocellulose and the raw material of leather gloss agent;The conduct in paint
Nitro spray painting, the solvent for printing ink, cellulose esters, fluorescent paint.
The method industrially generallyd use is sulphur acid as catalyst, intermittent esterification dehydration technique.Sulfuric acid is catalyzed
Agent has ideal catalytic activity, cheap, but corrosivity is strong and easily causes the side reactions such as oxidation, carbonization, polymerization, dehydration,
Product needs neutralized processing and Waste Sulfuric Acid to will cause environmental pollution.
Ethylene glycol in process of production can by-product one kind containing the impurity about 10% such as 1,2- butanediol, contain ethylene glycol about 30%,
Remaining is the waste material of water, and this waste material is taken as dangerous waste processing.This waste material cannot bring benefits, in addition need to take out ask it is other
Company's processing, causes the waste of ethylene glycol, brings economic benefit decline and environmental protection pressure.
Summary of the invention
The technical problem to be solved by the present invention is to be directed to the deficiencies in the prior art, and provide a kind of using low dense
Spend the device and method of ethylene glycol production high concentration glycol acetate.The device and method are with acetic acid and low concentration ethylene glycol
For raw material, wherein ethylene glycol content is 20% or more in low concentration ethylene glycol, it is particularly possible to is generated in ethylene glycol production process
One kind waste material containing ethylene glycol, be it is a kind of using low concentration ethylene glycol production high concentration glycol acetate technology.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of device using low concentration ethylene glycol production high concentration glycol acetate, including sequentially connected preheating
Device, fixed bed reactors, catalytic distillation tower, weight-removing column, lightness-removing column, treating column, it is characterised in that:
The preheater, be equipped with inlet and outlet, in which: import is divided into two-way, all the way be capable of providing ethylene glycol
Device is connected, and another way is connected with the device for being capable of providing acetic acid;
The fixed bed reactors, top is equipped with feed inlet I, bottom is equipped with discharge port I, in which: feed inlet I and preheating
The outlet of device is connected;
The catalytic distillation tower, top is equipped with exhaust outlet I, bottom is equipped with discharge port II, and the middle and upper part of tower wall side is set
There are feed inlet II, middle and lower part to be equipped with feed inlet III, the top of the tower wall other side is equipped with refluxing opening I, in which: feed inlet II and solid
The discharge port I of fixed bed reactor is connected;Feed inlet III is connected with the device that can provide acetic acid, supplements into tower excessive
Acetic acid;Exhaust outlet I is connected with condenser I and return tank I, and the outlet of return tank I is divided into two-way, wherein all the way with refluxing opening I phase
Connection, another way are connected with acetic acid recyclable device;
The weight-removing column, top is equipped with exhaust outlet II, bottom is equipped with discharge port III, the middle part of tower wall side be equipped with into
Material mouth IV, the tower wall other side top be equipped with refluxing opening II, in which: feed inlet IV point is two-way, wherein all the way with catalytic distillation
The discharge port II of tower is connected, and the second tunnel is connected with treating column;Exhaust outlet II is connected with condenser II and return tank II, reflux
The outlet of tank II is divided into two-way, wherein being connected all the way with refluxing opening II, the second tunnel is connected with lightness-removing column;Discharge port III with
Heavy substance storage tank is connected;
The lightness-removing column, top is equipped with exhaust outlet III, bottom is equipped with discharge port IV, the middle part of tower wall side be equipped with into
The top of material mouth V, the tower wall other side are equipped with refluxing opening III, in which: feed inlet V is connected with the second tunnel of return tank II;Exhaust
Mouthful III is connected with condenser III and return tank III, and the outlet of return tank III is divided into two-way, wherein all the way with refluxing opening III phase
Connection, the second tunnel is connected with the device for being capable of providing acetic acid
The treating column, top is equipped with exhaust outlet IV, bottom is equipped with discharge port V, and the middle part of tower wall side is equipped with charging
The top of mouth VI, the tower wall other side are equipped with refluxing opening IV, in which: feed inlet VI is connected with the discharge port IV of lightness-removing column;Exhaust
Mouth IV is connected with condenser IV and return tank IV, and the outlet of return tank IV is divided into two-way, wherein be connected all the way with refluxing opening IV,
Second tunnel is connected with product storage tank;Discharge port V is connected with the second tunnel of weight-removing column feed inlet IV.
In above-mentioned technical proposal, the fixed bed reactors, inside is filled with catalyst A;The catalyst A is solid
Body acid catalyst, preferably macropore Sulfonic acid cation resin catalyst.
In above-mentioned technical proposal, the catalytic distillation tower, catalytic section is filled with catalyst B;The catalyst B is solid
Body acid catalyst, preferably macropore Sulfonic acid cation resin catalyst.
In above-mentioned technical proposal, the preheater, fixed bed reactors, catalytic distillation tower, weight-removing column, lightness-removing column, essence
Tower processed is equipment of the existing technology or commercial equipment.
The present invention provides a kind of method using low concentration ethylene glycol production high concentration glycol acetate, including following
Step:
(1) fixed bed esterification: is passed by feed inlet I after low concentration ethylene glycol raw material and the preheated device heating of acetic acid
In reactor, esterification is carried out under the catalytic action of the catalyst A of acetic acid and ethylene glycol in fixed bed reactors, is obtained just
Order reaction product;Primary reaction product enters in catalytic distillation tower followed by discharge port I, feed inlet II;
(2) catalytic distillation reacts: the primary reaction product formed in fixed bed reactors enters in catalytic distillation tower, In
Catalytic distillation reaction is carried out under the catalytic action of catalyst B in catalytic distillation tower, and is separated;Tower top obtains light group after separation
Point, light component is water and acetic acid, condenses the water for obtaining liquid through condenser I after exhaust outlet I discharge and acetic acid enters reflux
Tank I;Material a part is returned in catalytic distillation tower from refluxing opening I and is recycled in return tank I, and another part and acetic acid recycling fill
It sets and is connected;Tower bottom obtains whole order reaction product after separation, and whole order reaction product is glycol acetate, low concentration ethylene glycol
The mixture of partial impurities, micro ethylene glycol and micro-acetic acid in raw material, followed by entering after discharge port II, feed inlet IV
Into weight-removing column;During carrying out catalytic distillation reaction, fresh, excessive acetic acid is imported from feed inlet III, is conducive to
It reacts and is carried out to the direction for generating glycol acetate;
(3) take off weight: the whole order reaction product of catalytic distillation tower tower bottom enters in weight-removing column, is divided in weight-removing column
From tower top obtains light component, and light component is gaseous state glycol acetate, acetic acid and micro heavy constituent, is discharged from exhaust outlet II
Liquid is condensed by condenser II and enters return tank II, and material a part returns to weight-removing column by refluxing opening II in return tank II
In recycle, another part by feed inlet V be sent into lightness-removing column in;The heavy substance being discharged from tower bottom discharge port III is low dense
Spend the partial impurities in ethylene glycol raw material and a small amount of ethylene glycol and acetic acid;
(4) it takes off light: after the material of weight-removing column tower top enters in lightness-removing column, being separated in lightness-removing column, tower top obtains
Light component, light component are gaseous state acetic acid and micro glycol acetate, are condensed after exhaust outlet III discharge through condenser III
Enter return tank III for liquid, material a part is returned in lightness-removing column by refluxing opening III and recycled in return tank III, separately
A part is connected with the device for being capable of providing acetic acid;The material being discharged from tower bottom discharge port IV is mainly ethylene glycol diacetic acid,
Remaining is partial impurities and micro ethylene glycol in micro material ethylene glycol, passes through feed inlet VI and is sent into treating column;
(5) refine: the material of lightness-removing column tower bottom enters in treating column, is separated in treating column, and tower top obtains gently
Component, light component are gaseous state glycol acetate, are condensed into liquid through condenser IV after exhaust outlet IV discharge and enter reflux
Material a part is returned in treating column by refluxing opening IV and is recycled in tank IV, return tank IV, and another part and ethylene glycol are double
Acetic acid esters product storage tank is connected;The heavy substance being discharged from tower bottom discharge port V is the partial impurities and second two in raw material ethylene glycol
Alcohol is back to circular treatment in weight-removing column by feed inlet IV.
In above-mentioned technical proposal, in step (1), the low concentration ethylene glycol raw material is to generate in ethylene glycol production process
The waste material containing ethylene glycol, wherein glycol concentration be not less than 20%.
In above-mentioned technical proposal, in step (1), mole of ethylene glycol and acetic acid in the low concentration ethylene glycol raw material
Than for 1:1~3, preferably 1:2.2~2.6.
In above-mentioned technical proposal, in step (1), the low concentration ethylene glycol raw material and the preheated device of acetic acid are heated to
It is passed into fixed bed reactors after 60-80 DEG C, air speed is 0.5~2h-1。
In above-mentioned technical proposal, in step (1), the esterification condition are as follows: temperature is 60~80 DEG C, and pressure is
0.6~1.2Mpa;Temperature is preferably 65~70 DEG C, and pressure is preferably 0.7~0.9Mpa.
In above-mentioned technical proposal, in step (1), the catalyst A is solid acid catalyst, preferably macropore sulfonic acid sun
Ion exchange resin catalyst.
In above-mentioned technical proposal, in step (2), the primary reaction product formed in fixed bed reactors enters catalysis and steams
Evaporating the air speed in tower is 0.5-3h-1。
In above-mentioned technical proposal, in step (2), the catalyst B is solid acid catalyst, preferably macropore sulfonic acid sun
Ion exchange resin catalyst.
In above-mentioned technical proposal, in step (2), the catalytic distillation reaction, reaction condition are as follows: reaction temperature 100
~120 DEG C, reaction pressure is 0.10~0.20Mpa.
In above-mentioned technical proposal, in step (2), the catalytic distillation tower, operating condition are as follows: tower top temperature be 80~
120 DEG C, pressure is 0.10~0.15Mpa;Column bottom temperature is 160~170 DEG C, and pressure is 0.15~0.35Mpa.
In above-mentioned technical proposal, in step (2), fresh, the excessive acetic acid importeding into catalytic distillation tower, with step
(1) molar ratio that the acetic acid in preheater is imported into is 1~3:1, preferably 1.5-2:1.
In above-mentioned technical proposal, in step (2), the reflux, reflux ratio is 0.5~3.
In above-mentioned technical proposal, in step (3), the weight-removing column, operating condition are as follows: tower top temperature is 110~120
DEG C, pressure be 0.10~0.15Mpa, column bottom temperature is 200~220 DEG C, pressure is 0.25~0.35Mpa.
In above-mentioned technical proposal, in step (3), the reflux, reflux ratio is 0.3~2.
In above-mentioned technical proposal, in step (4), the lightness-removing column, operating condition are as follows: tower top temperature is 110~120
DEG C, pressure be 0.10~0.15Mpa, column bottom temperature is 180~190 DEG C, pressure is 0.25~0.35MPa.
In above-mentioned technical proposal, in step (4), the reflux, reflux ratio is 0.5~3.
In above-mentioned technical proposal, in step (5), the treating column, operating condition are as follows: tower top temperature is 110~120
DEG C, pressure be 0.03~0.10Mpa, column bottom temperature is 150~170 DEG C, pressure is 0.10~0.25Mpa.
In above-mentioned technical proposal, in step (5), the reflux, reflux ratio is 0.3~2.
The advantages of technical solution of the present invention, is:
(1) raw material ethylene glycol of the invention can be the waste material generated in ethylene glycol production process, which is dangerous waste, this
Kind waste material cannot bring benefits, or even need to take out and other company is asked to handle, and cause the waste of ethylene glycol, bring under economic benefit
Drop and environmental protection pressure, so the present invention has apparent economic benefit and environment-friendly advantage.
(2) raw material ethylene glycol of the invention is of less demanding to the concentration of ethylene glycol, and glycol concentration is not less than 20%.
(3) product quality of the invention is excellent: concentration >=99.0% of glycol acetate, ethylene glycol acetate concentration
≤ 1.0%, water≤0.1%, acetic acid≤0.2%.
Detailed description of the invention
Fig. 1: the process flow chart of the method for the present invention;
Fig. 2: the overall structure diagram of apparatus of the present invention;
Wherein: 1 is preheater, and 2 be fixed bed reactors, and 3 be catalytic distillation tower, and 4 be weight-removing column, and 5 be lightness-removing column, and 6 are
Treating column.
Specific embodiment
The specific embodiment of technical solution of the present invention is described in detail below, but the present invention is not limited in being described below
Hold:
The present invention provides a kind of device using low concentration ethylene glycol production high concentration glycol acetate, including successively
Preheater 1, fixed bed reactors 2, catalytic distillation tower 3, the weight-removing column 4 of connection, lightness-removing column 5, treating column 6, as shown in Figure 2:
The preheater, be equipped with inlet and outlet, in which: import is divided into two-way, all the way be capable of providing ethylene glycol
Device is connected, and another way is connected with the device for being capable of providing acetic acid;
The fixed bed reactors, top is equipped with feed inlet I, bottom is equipped with discharge port I, in which: feed inlet I and preheating
The outlet of device is connected;
The catalytic distillation tower, top is equipped with exhaust outlet I, bottom is equipped with discharge port II, and the middle and upper part of tower wall side is set
There are feed inlet II, middle and lower part to be equipped with feed inlet III, the top of the tower wall other side is equipped with refluxing opening I, in which: feed inlet II and solid
The discharge port I of fixed bed reactor is connected;Feed inlet III is connected with the device that can provide acetic acid, supplements into tower excessive
Acetic acid;Exhaust outlet I is connected with condenser I and return tank I, and the outlet of return tank I is divided into two-way, wherein all the way with refluxing opening I phase
Connection, another way are connected with acetic acid recyclable device;
The weight-removing column, top is equipped with exhaust outlet II, bottom is equipped with discharge port III, the middle part of tower wall side be equipped with into
Material mouth IV, the tower wall other side top be equipped with refluxing opening II, in which: feed inlet IV point is two-way, wherein all the way with catalytic distillation
The discharge port II of tower is connected, and the second tunnel is connected with treating column;Exhaust outlet II is connected with condenser II and return tank II, reflux
The outlet of tank II is divided into two-way, wherein being connected all the way with refluxing opening II, the second tunnel is connected with lightness-removing column;Discharge port III with
Heavy substance storage tank is connected;
The lightness-removing column, top is equipped with exhaust outlet III, bottom is equipped with discharge port IV, the middle part of tower wall side be equipped with into
The top of material mouth V, the tower wall other side are equipped with refluxing opening III, in which: feed inlet V is connected with the second tunnel of return tank II;Exhaust
Mouthful III is connected with condenser III and return tank III, and the outlet of return tank III is divided into two-way, wherein all the way with refluxing opening III phase
Connection, the second tunnel is connected with the device for being capable of providing acetic acid;
The treating column, top is equipped with exhaust outlet IV, bottom is equipped with discharge port V, and the middle part of tower wall side is equipped with charging
The top of mouth VI, the tower wall other side are equipped with refluxing opening IV, in which: feed inlet VI is connected with the discharge port IV of lightness-removing column;Exhaust
Mouth IV is connected with condenser IV and return tank IV, and the outlet of return tank IV is divided into two-way, wherein be connected all the way with refluxing opening IV,
Second tunnel is connected with product storage tank;Discharge port V is connected with the second tunnel of weight-removing column feed inlet IV;
The fixed bed reactors, inside are filled with catalyst A;The catalyst A is solid acid catalyst, preferably
For macropore Sulfonic acid cation resin catalyst;
The catalytic distillation tower, catalytic section are filled with catalyst B;The catalyst B is solid acid catalyst, preferably
For macropore Sulfonic acid cation resin catalyst.
In the present invention, the preheater, fixed bed reactors, catalytic distillation tower, weight-removing column, lightness-removing column, treating column is equal
For equipment of the existing technology or commercial equipment.
The present invention provides a kind of method using low concentration ethylene glycol production high concentration glycol acetate, and flow chart is such as
Shown in Fig. 1, comprising the following steps:
(1) fixed bed esterification: is passed by feed inlet I after low concentration ethylene glycol raw material and the preheated device heating of acetic acid
In reactor (2), esterification is carried out under the catalytic action of the catalyst A of acetic acid and ethylene glycol in fixed bed reactors, is obtained
To primary reaction product;Primary reaction product enters in catalytic distillation tower followed by discharge port I, feed inlet II;
(2) catalytic distillation reacts: the primary reaction product formed in fixed bed reactors enters in catalytic distillation tower, In
Catalytic distillation reaction is carried out under the catalytic action of catalyst B in catalytic distillation tower, and is separated;Tower top obtains light group after separation
Point, light component is water and acetic acid, condenses the water for obtaining liquid through condenser I after exhaust outlet I discharge and acetic acid enters reflux
Tank I;Material a part is returned in catalytic distillation tower from refluxing opening I and is recycled in return tank I, and another part and acetic acid recycling fill
It sets and is connected;Tower bottom obtains whole order reaction product after separation, and whole order reaction product is glycol acetate, low concentration ethylene glycol
The mixture of partial impurities, micro ethylene glycol and micro-acetic acid in raw material, followed by entering after discharge port II, feed inlet IV
Into weight-removing column;During carrying out catalytic distillation reaction, fresh, excessive acetic acid is imported from feed inlet III, is conducive to
It reacts and is carried out to the direction for generating glycol acetate;
(3) take off weight: the whole order reaction product of catalytic distillation tower tower bottom enters in weight-removing column, is divided in weight-removing column
From tower top obtains light component, and light component is gaseous state glycol acetate, acetic acid and micro heavy constituent, is discharged from exhaust outlet II
Liquid is condensed by condenser II and enters return tank II, and material a part returns to weight-removing column by refluxing opening II in return tank II
In recycle, another part by feed inlet V be sent into lightness-removing column in;The heavy substance being discharged from tower bottom discharge port III is low dense
Spend the partial impurities in ethylene glycol raw material and a small amount of ethylene glycol and acetic acid;
(4) it takes off light: after the material of weight-removing column tower top enters in lightness-removing column, being separated in lightness-removing column, tower top obtains
Light component, light component are gaseous state acetic acid and micro glycol acetate, are condensed after exhaust outlet III discharge through condenser III
Enter return tank III for liquid, material a part is returned in lightness-removing column by refluxing opening III and recycled in return tank III, separately
A part is connected with the device for being capable of providing acetic acid;The material being discharged from tower bottom discharge port IV is mainly ethylene glycol diacetic acid,
Remaining is partial impurities and micro ethylene glycol in micro material ethylene glycol, passes through feed inlet VI and is sent into treating column;
(5) refine: the material of lightness-removing column tower bottom enters in treating column, is separated in treating column, and tower top obtains gently
Component, light component are gaseous state glycol acetate, are condensed into liquid through condenser IV after exhaust outlet IV discharge and enter reflux
Material a part is returned in treating column by refluxing opening IV and is recycled in tank IV, return tank IV, and another part and ethylene glycol are double
Acetic acid esters product storage tank is connected;The heavy substance being discharged from tower bottom discharge port V is the partial impurities and second two in raw material ethylene glycol
Alcohol is back to circular treatment in weight-removing column by feed inlet IV.
The present invention is illustrated below with reference to specific embodiment:
Embodiment 1:
A method of high concentration glycol acetate being produced using low concentration ethylene glycol, specifically includes the following steps:
(1) esterification: after acetic acid and the preheated device of ethylene glycol (molar ratio 2.4:1) are heated to be 65-70 DEG C, by feeding
Mouth I is passed into fixed bed reactors, air speed 0.8h-1, the catalyst A of acetic acid and ethylene glycol in fixed bed reactors
Esterification is carried out under conditions of 65~70 DEG C, 0.7~0.8Mpa under catalytic action, obtains primary reaction product;It is primary anti-
Product is answered to enter in catalytic distillation tower followed by discharge port I, feed inlet II;
The ethylene glycol raw material is the waste material generated in ethylene glycol production process, and wherein glycol concentration is 30%, no
The heavy substance concentration 10% of reaction is participated in, remaining is water;
The catalyst A is macropore Sulfonic acid cation resin catalyst, using triumphant auspicious environmentally friendly Science and Technology Co., Ltd.
KC156 type ethylene acetate catalyst.
(2) catalytic distillation reacts: primary reaction product (the air speed 2h formed in fixed bed reactors-1) enter catalysis
In destilling tower, under the catalytic action of the catalyst B in catalytic distillation tower, conversion zone is in 100~110 DEG C, 0.10~0.15MPa
Operating condition under, carry out catalytic distillation reaction, and separated;Tower top obtains light component after separation, and light component is water (quality hundred
Score 20%) and acetic acid (mass percent 80%), liquid, which is condensed into, through condenser after exhaust outlet I discharge enters reflux
Tank;Material a part returns to recycling, another part and acetic acid recyclable device in catalytic distillation tower from refluxing opening I in return tank
It is connected;Tower bottom obtains whole order reaction product after separation, and whole order reaction product is glycol acetate, in raw material ethylene glycol
Partial impurities, about 30% acetic acid and the mixture of a small amount of ethylene glycol enter de- weight followed by discharge port II, feed inlet IV
In tower;During carrying out catalytic distillation reaction, fresh, excessive acetic acid is imported from feed inlet III, in step (1)
The molar ratio for importing the acetic acid in preheater is 1.8:1.
The catalyst B is macropore Sulfonic acid cation resin catalyst, using triumphant auspicious environmentally friendly Science and Technology Co., Ltd.
KC156-BD type ethylene acetate module catalyst;
The tower top operating condition of the catalytic distillation tower: temperature is 85~90 DEG C, and pressure is 0.10~0.15MPa, tower
Bottom operating condition: temperature is 165~170 DEG C, and pressure is 0.25~0.30MPa;
The reflux ratio of the catalytic distillation tower is 1.
(3) take off weight: the whole order reaction product of catalytic distillation tower tower bottom enters in weight-removing column, after being separated in weight-removing column,
Tower top obtains light component, and light component is gaseous state glycol acetate, acetic acid and micro heavy constituent, passes through after exhaust outlet II discharge
Condenser is condensed into liquid and enters return tank, and material a part is returned by refluxing opening II and recycles benefit in weight-removing column in return tank
With another part is sent into lightness-removing column by feed inlet V;The heavy substance being discharged from tower bottom discharge port III is in raw material ethylene glycol
Partial impurities, about 5% acetic acid and ethylene glycol.
The tower top operating condition of the weight-removing column: temperature is 110~115 DEG C, and pressure is 0.10~0.15MPa, tower bottom
Operating condition: temperature is 200~210 DEG C, and pressure is 0.25~0.30MPa;
The reflux ratio of the weight-removing column is 0.6.
(4) take off light: the material of weight-removing column tower top enters in lightness-removing column, and after separating in lightness-removing column, tower top obtains light group
Point, light component be gaseous state acetic acid and micro glycol acetate, from exhaust outlet III discharge after through condenser be condensed into liquid into
Enter return tank, material a part is returned in lightness-removing column by refluxing opening III and recycled in return tank, and another part and acetic acid are former
Batch can is connected;The material being discharged from tower bottom discharge port IV is mainly ethylene glycol diacetic acid, remaining is in micro material ethylene glycol
Partial impurities and micro ethylene glycol by feed inlet VI be sent into treating column.
The tower top operating condition of the lightness-removing column: temperature is 110~115 DEG C, and pressure is 0.10~0.15Mpa, tower bottom
Operating condition: temperature is 180~185 DEG C, and pressure is 0.25~0.30Mpa;
The reflux ratio of the lightness-removing column is 1.5.
(5) refine: the material of lightness-removing column tower bottom enters in treating column, and after separating in treating column, tower top obtains light group
Point, light component is gaseous state glycol acetate, is condensed into liquid through condenser after exhaust outlet II discharge and enters return tank, returns
Material a part is returned in treating column by refluxing opening IV in stream tank recycles, another part and glycol acetate product
Storage tank is connected;The heavy substance being discharged from tower bottom discharge port V is that the partial impurities and ethylene glycol in raw material ethylene glycol pass through charging
Mouth IV is sent into weight-removing column processing.
The tower top operating condition of the treating column: temperature is 110~115 DEG C, and pressure is 0.03~0.05Mpa, tower bottom
Operating condition: temperature is 150~155 DEG C, and pressure is 0.10~0.15Mpa;
The reflux ratio of the treating column is 0.8.
In the present embodiment product, the concentration of glycol acetate is 99.1%, and ethylene glycol acetate concentration is
0.66%, the concentration of water is 0.09%, and the concentration of acetic acid is 0.15%.
Embodiment 2:
A method of high concentration glycol acetate being produced using low concentration ethylene glycol, specifically includes the following steps:
(1) esterification: after acetic acid and the preheated device of ethylene glycol (molar ratio 2.4:1) are heated to be 65-70 DEG C, by feeding
Mouth I is passed into fixed bed reactors, air speed 0.8h-1, the catalyst A of acetic acid and ethylene glycol in fixed bed reactors
Esterification is carried out under conditions of 65~70 DEG C, 0.7~0.8MPa under catalytic action, obtains primary reaction product;It is primary anti-
Product is answered to enter in catalytic distillation tower followed by discharge port I, feed inlet II;
The ethylene glycol raw material is the waste material generated in ethylene glycol production process, and wherein glycol concentration is 50%, no
The heavy substance concentration 10% of reaction is participated in, remaining is water;
The catalyst A is macropore Sulfonic acid cation resin catalyst, using triumphant auspicious environmentally friendly Science and Technology Co., Ltd.
KC156 type ethylene acetate catalyst.
(2) catalytic distillation reacts: the primary reaction product (1.5h formed in fixed bed reactors-1) enter catalytic distillation
In tower, under the catalytic action of the catalyst B in catalytic distillation tower, conversion zone is in 100~110 DEG C, the behaviour of 0.10~0.15MPa
Under the conditions of work, catalytic distillation reaction is carried out, and separated;Tower top obtains light component after separation, and light component is water (mass percent
20%) with acetic acid (mass percent 80%), liquid is condensed into through condenser after exhaust outlet I discharge and enters return tank;It returns
Material a part is recycled from refluxing opening I return catalytic distillation tower in stream tank, another part is connected with acetic acid recyclable device
It connects;Tower bottom obtains whole order reaction product after separation, and whole order reaction product is glycol acetate, the part in raw material ethylene glycol
Impurity, about 30% acetic acid and the mixture of a small amount of ethylene glycol enter weight-removing column followed by discharge port II, feed inlet IV
In;During carrying out catalytic distillation reaction, fresh, excessive acetic acid is imported from feed inlet III, and is led in step (1)
The molar ratio for entering the acetic acid in preheater is 1.8:1.
The catalyst B is macropore Sulfonic acid cation resin catalyst, using triumphant auspicious environmentally friendly Science and Technology Co., Ltd.
KC156-BD type ethylene acetate module catalyst;
The tower top operating condition of the catalytic distillation tower: temperature is 85~90 DEG C, and pressure is 0.10~0.15MPa, tower
Bottom operating condition: temperature is 165~170 DEG C, and pressure is 0.25~0.30MPa;
The reflux ratio of the catalytic distillation tower is 0.9.
(3) take off weight: the whole order reaction product of catalytic distillation tower tower bottom enters in weight-removing column, after being separated in weight-removing column,
Tower top obtains light component, and light component is gaseous state glycol acetate, acetic acid and micro heavy constituent, passes through after exhaust outlet II discharge
Condenser is condensed into liquid and enters return tank, and material a part is returned by refluxing opening II and recycles benefit in weight-removing column in return tank
With another part is sent into lightness-removing column by feed inlet V;The heavy substance being discharged from tower bottom discharge port III is in raw material ethylene glycol
Partial impurities, about 5% acetic acid and ethylene glycol.
The tower top operating condition of the weight-removing column: temperature is 110~115 DEG C, and pressure is 0.10~0.15MPa, tower bottom
Operating condition: temperature is 200~210 DEG C, and pressure is 0.25~0.30MPa;
The reflux ratio of the weight-removing column is 0.6.
(4) take off light: the material of weight-removing column tower top enters in lightness-removing column, and after separating in lightness-removing column, tower top obtains light group
Point, light component be gaseous state acetic acid and micro glycol acetate, from exhaust outlet III discharge after through condenser be condensed into liquid into
Enter return tank, material a part is returned in lightness-removing column by refluxing opening III and recycled in return tank, and another part and acetic acid are former
Batch can is connected;The material being discharged from tower bottom discharge port IV is mainly ethylene glycol diacetic acid, remaining is in micro material ethylene glycol
Partial impurities and micro ethylene glycol by feed inlet VI be sent into treating column.
The tower top operating condition of the lightness-removing column: temperature is 110~115 DEG C, and pressure is 0.10~0.15Mpa, tower bottom
Operating condition: temperature is 180~185 DEG C, and pressure is 0.25~0.30Mpa;
The reflux ratio of the lightness-removing column is 1.5.
(5) refine: the material of lightness-removing column tower bottom enters in treating column, and after separating in treating column, tower top obtains light group
Point, light component is gaseous state glycol acetate, is condensed into liquid through condenser after exhaust outlet II discharge and enters return tank, returns
Material a part is returned in treating column by refluxing opening IV in stream tank recycles, another part and glycol acetate product
Storage tank is connected;The heavy substance being discharged from tower bottom discharge port V is that the partial impurities and ethylene glycol in raw material ethylene glycol pass through charging
Mouth IV is sent into weight-removing column processing.
The tower top operating condition of the treating column: temperature is 110~115 DEG C, and pressure is 0.03~0.05Mpa, tower bottom
Operating condition: temperature is 150~155 DEG C, and pressure is 0.10~0.15Mpa;
The reflux ratio of the treating column is 0.8.
In the present embodiment product, the concentration of glycol acetate is 99.3%, and ethylene glycol acetate concentration is
0.60%, the concentration of water is 0.04%, and the concentration of acetic acid is 0.06%.
Examples detailed above is technical conception and technical characteristics to illustrate the invention, can not be limited with this of the invention
Protection scope.The equivalent transformation or modification that all essence according to the present invention is done, should all cover in protection scope of the present invention
Within.
Claims (10)
1. a kind of method using low concentration ethylene glycol production high concentration glycol acetate, which is characterized in that including following
Step:
(1) fixed bed esterification: is passed by feed inlet I after low concentration ethylene glycol raw material and the preheated device of acetic acid (1) heating
In reactor (2), esterification is carried out under the catalytic action of the catalyst A of acetic acid and ethylene glycol in fixed bed reactors, is obtained
To primary reaction product;Primary reaction product enters in catalytic distillation tower (3) followed by discharge port I, feed inlet II;
(2) catalytic distillation reacts: the primary reaction product formed in fixed bed reactors enters in catalytic distillation tower, is being catalyzed
Catalytic distillation reaction is carried out under the catalytic action of catalyst B in destilling tower, and is separated;Tower top obtains light component after separation,
Light component is water and acetic acid, condenses the water for obtaining liquid through condenser I after exhaust outlet I discharge and acetic acid enters return tank I;
Material a part is returned in catalytic distillation tower from refluxing opening I and is recycled in return tank I, another part and acetic acid recyclable device phase
Connection;Tower bottom obtains whole order reaction product after separation, and whole order reaction product is glycol acetate, low concentration ethylene glycol raw material
In partial impurities, micro ethylene glycol and micro-acetic acid mixture, it is de- followed by being entered after discharge port II, feed inlet IV
In weight tower;During carrying out catalytic distillation reaction, fresh, excessive acetic acid is imported from feed inlet III, is conducive to react
It is carried out to the direction for generating glycol acetate;
(3) take off weight: the whole order reaction product of catalytic distillation tower tower bottom enters in weight-removing column, is separated in weight-removing column, tower
Top obtains light component, and light component is gaseous state glycol acetate, acetic acid and micro heavy constituent, through cold after exhaust outlet II discharge
Condenser II is condensed into liquid and enters return tank II, and material a part is returned in weight-removing column by refluxing opening II and recycled in return tank II
It utilizes, another part is sent into lightness-removing column by feed inlet V;The heavy substance being discharged from tower bottom discharge port III is low concentration second two
Partial impurities and a small amount of ethylene glycol and acetic acid in raw polyol;
(4) it takes off light: after the material of weight-removing column tower top enters in lightness-removing column, being separated in lightness-removing column, tower top obtains light group
Point, light component is gaseous state acetic acid and micro glycol acetate, is condensed into liquid through condenser III after exhaust outlet III discharge
State enters return tank III, and material a part is returned in lightness-removing column by refluxing opening III and recycled in return tank III, another portion
Divide and is connected with the device for being capable of providing acetic acid;The material being discharged from tower bottom discharge port IV is mainly ethylene glycol diacetic acid, remaining
For in micro material ethylene glycol partial impurities and micro ethylene glycol, pass through feed inlet VI be sent into treating column;
(5) refine: the material of lightness-removing column tower bottom enters in treating column, is separated in treating column, and tower top obtains light component,
Light component is gaseous state glycol acetate, is condensed into liquid through condenser IV after exhaust outlet IV discharge and enters return tank IV,
Material a part is returned in treating column by refluxing opening IV and is recycled in return tank IV, another part and glycol acetate
Product storage tank is connected;The heavy substance being discharged from tower bottom discharge port V is that the partial impurities and ethylene glycol in raw material ethylene glycol pass through
Feed inlet IV is back to circular treatment in weight-removing column.
2. the method for production high concentration glycol acetate according to claim 1, it is characterised in that: in step (1),
The low concentration ethylene glycol raw material is the waste material containing ethylene glycol generated in ethylene glycol production process, wherein glycol concentration
Not less than 20%;The molar ratio of ethylene glycol and acetic acid in the low concentration ethylene glycol raw material is 1:1~3.
3. the method for production high concentration glycol acetate according to claim 1, it is characterised in that: in step (1),
The low concentration ethylene glycol raw material and the preheated device of acetic acid are passed into fixed bed reactors after being heated to 60-80 DEG C, air speed
For 0.5~2h-1;The esterification condition are as follows: temperature is 60~80 DEG C, and pressure is 0.6~1.2Mpa.
4. the method for production high concentration glycol acetate according to claim 1, it is characterised in that: in step (2),
It is 0.5-3h that the primary reaction product formed in fixed bed reactors, which enters the air speed in catalytic distillation tower,-1;The catalysis
Distillation reaction, reaction condition are as follows: reaction temperature is 100~120 DEG C, and reaction pressure is 0.10~0.20Mpa;The reflux,
Reflux ratio is 0.5~3.
5. the method for production high concentration glycol acetate according to claim 1, it is characterised in that: in step (2)
Fresh, the excessive acetic acid importeding into catalytic distillation tower, the molar ratio with the acetic acid being imported into step (1) in preheater
For 1~3:1;Catalyst A described in step (1) is solid acid catalyst, and catalyst B described in step (2) is solid acid
Catalyst.
6. the method for production high concentration glycol acetate according to claim 1, it is characterised in that: in step (3),
The weight-removing column, operating condition are as follows: tower top temperature is 110~120 DEG C, pressure is 0.10~0.15Mpa, and column bottom temperature is
200~220 DEG C, pressure be 0.25~0.35Mpa;The reflux, reflux ratio are 0.3~2.
7. the method for production high concentration glycol acetate according to claim 1, it is characterised in that: in step (4),
The lightness-removing column, operating condition are as follows: tower top temperature is 110~120 DEG C, pressure is 0.10~0.15Mpa, and column bottom temperature is
180~190 DEG C, pressure be 0.25~0.35Mpa;The reflux, reflux ratio are 0.5~3.
8. the method for production high concentration glycol acetate according to claim 1, it is characterised in that: in step (5),
The treating column, operating condition are as follows: tower top temperature is 110~120 DEG C, pressure is 0.03~0.10Mpa, and column bottom temperature is
150~170 DEG C, pressure be 0.10~0.25Mpa;The reflux, reflux ratio are 0.3~2.
9. a kind of device using low concentration ethylene glycol production high concentration glycol acetate, including sequentially connected preheater
(1), fixed bed reactors (2), catalytic distillation tower (3), weight-removing column (4), lightness-removing column (5), treating column (6), it is characterised in that:
The preheater (1) is equipped with inlet and outlet, in which: import is divided into two-way, all the way with the dress that is capable of providing ethylene glycol
It sets and is connected, another way is connected with the device for being capable of providing acetic acid;
The fixed bed reactors (2), top is equipped with feed inlet I, bottom is equipped with discharge port I, in which: feed inlet I and preheating
The outlet of device is connected;
The catalytic distillation tower (3), top is equipped with exhaust outlet I, bottom is equipped with discharge port II, and the middle and upper part of tower wall side is equipped with
Feed inlet II, middle and lower part are equipped with feed inlet III, and the top of the tower wall other side is equipped with refluxing opening I, in which: feed inlet II and fixation
The discharge port I of bed reactor is connected;Feed inlet III is connected with the device that can provide acetic acid, and excessive second is supplemented into tower
Acid;Exhaust outlet I is connected with condenser I and return tank I, and the outlet of return tank I is divided into two-way, wherein being connected all the way with refluxing opening I
It connects, another way is connected with acetic acid recyclable device;
The weight-removing column (4), top is equipped with exhaust outlet II, bottom is equipped with discharge port III, and the middle part of tower wall side is equipped with charging
Mouthful IV, the tower wall other side top be equipped with refluxing opening II, in which: feed inlet IV points are two-way, wherein all the way with catalytic distillation tower
Discharge port II be connected, the second tunnel is connected with treating column (6);Exhaust outlet II is connected with condenser II and return tank II, returns
The outlet of stream tank II is divided into two-way, wherein being connected all the way with refluxing opening II, the second tunnel is connected with lightness-removing column;Discharge port III
It is connected with heavy substance storage tank;
The lightness-removing column (5), top is equipped with exhaust outlet III, bottom is equipped with discharge port IV, and the middle part of tower wall side is equipped with charging
The top of mouth V, the tower wall other side are equipped with refluxing opening III, in which: feed inlet V is connected with the second tunnel of return tank II;Exhaust outlet
III is connected with condenser III and return tank III, and the outlet of return tank III is divided into two-way, wherein being connected all the way with refluxing opening III
It connects, the second tunnel is connected with the device for being capable of providing acetic acid;
The treating column (6), top is equipped with exhaust outlet IV, bottom is equipped with discharge port V, and the middle part of tower wall side is equipped with feed inlet
The top of VI, the tower wall other side are equipped with refluxing opening IV, in which: feed inlet VI is connected with the discharge port IV of lightness-removing column;Exhaust outlet
IV is connected with condenser IV and return tank IV, and the outlet of return tank IV is divided into two-way, wherein be connected all the way with refluxing opening IV, the
Two tunnels are connected with product storage tank;Discharge port V is connected with the second tunnel of weight-removing column feed inlet IV.
10. the device of production high concentration glycol acetate according to claim 9, it is characterised in that: described consolidates
Fixed bed reactor, inside are filled with catalyst A, and catalyst A is solid acid catalyst;The catalytic distillation tower, catalytic section dress
It is filled with catalyst B, catalyst B is solid acid catalyst.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910874100.XA CN110423197B (en) | 2019-09-17 | 2019-09-17 | Device and method for producing ethylene glycol diacetate by using low-concentration ethylene glycol |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910874100.XA CN110423197B (en) | 2019-09-17 | 2019-09-17 | Device and method for producing ethylene glycol diacetate by using low-concentration ethylene glycol |
Publications (2)
Publication Number | Publication Date |
---|---|
CN110423197A true CN110423197A (en) | 2019-11-08 |
CN110423197B CN110423197B (en) | 2023-11-14 |
Family
ID=68418177
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201910874100.XA Active CN110423197B (en) | 2019-09-17 | 2019-09-17 | Device and method for producing ethylene glycol diacetate by using low-concentration ethylene glycol |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN110423197B (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111116361A (en) * | 2020-01-15 | 2020-05-08 | 凯瑞环保科技股份有限公司 | Device and method for preparing ethylene glycol diester by using waste chemical raw materials |
CN111574365A (en) * | 2020-06-15 | 2020-08-25 | 凯瑞环保科技股份有限公司 | Device and method for producing glycol diacrylate by using low-concentration ethylene glycol |
CN112608234A (en) * | 2020-12-30 | 2021-04-06 | 江苏盛叶欣化工新材料有限公司 | Method for producing high-content ethylene glycol diacetate and coproducing diethylene glycol diacetate |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN201862283U (en) * | 2010-09-27 | 2011-06-15 | 江阴博伦化纤有限公司 | Extracting device for ethanediol and acetaldehyde in esterification waste gas |
CN104045554A (en) * | 2014-07-09 | 2014-09-17 | 江苏天音化工有限公司 | Method for preparing ethylene glycol diacetate |
CN104355996A (en) * | 2014-09-30 | 2015-02-18 | 天津中昊天久工程技术有限公司 | Method for synthesizing ethylene glycol diacetate by adopting transesterification method |
WO2015026073A1 (en) * | 2013-08-20 | 2015-02-26 | Sk Innovation Co.,Ltd. | Method for preparing glycol ester using reactive distillation |
CN105130760A (en) * | 2015-08-10 | 2015-12-09 | 华南理工大学 | New technology for preparation of high purity MTBE |
CN106146303A (en) * | 2016-07-26 | 2016-11-23 | 江门谦信化工发展有限公司 | A kind of acetic acid mixes continuous process system and the method for butyl ester |
CN109369396A (en) * | 2018-11-30 | 2019-02-22 | 福州大学 | A kind of method that direct esterification prepares high-purity ethylene acetate |
CN210825997U (en) * | 2019-09-17 | 2020-06-23 | 凯瑞环保科技股份有限公司 | Device for producing ethylene glycol diacetate by using low-concentration ethylene glycol |
-
2019
- 2019-09-17 CN CN201910874100.XA patent/CN110423197B/en active Active
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN201862283U (en) * | 2010-09-27 | 2011-06-15 | 江阴博伦化纤有限公司 | Extracting device for ethanediol and acetaldehyde in esterification waste gas |
WO2015026073A1 (en) * | 2013-08-20 | 2015-02-26 | Sk Innovation Co.,Ltd. | Method for preparing glycol ester using reactive distillation |
CN104045554A (en) * | 2014-07-09 | 2014-09-17 | 江苏天音化工有限公司 | Method for preparing ethylene glycol diacetate |
CN104355996A (en) * | 2014-09-30 | 2015-02-18 | 天津中昊天久工程技术有限公司 | Method for synthesizing ethylene glycol diacetate by adopting transesterification method |
CN105130760A (en) * | 2015-08-10 | 2015-12-09 | 华南理工大学 | New technology for preparation of high purity MTBE |
CN106146303A (en) * | 2016-07-26 | 2016-11-23 | 江门谦信化工发展有限公司 | A kind of acetic acid mixes continuous process system and the method for butyl ester |
CN109369396A (en) * | 2018-11-30 | 2019-02-22 | 福州大学 | A kind of method that direct esterification prepares high-purity ethylene acetate |
CN210825997U (en) * | 2019-09-17 | 2020-06-23 | 凯瑞环保科技股份有限公司 | Device for producing ethylene glycol diacetate by using low-concentration ethylene glycol |
Non-Patent Citations (2)
Title |
---|
孙彦开: "煤制乙二醇废料回收及其合成高附加值聚氨酯产品的技术研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》, pages 016 - 580 * |
马江权等: "己二酸废料乙醇酯化反应动力学研究", vol. 23, no. 1, pages 9 - 11 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111116361A (en) * | 2020-01-15 | 2020-05-08 | 凯瑞环保科技股份有限公司 | Device and method for preparing ethylene glycol diester by using waste chemical raw materials |
CN111574365A (en) * | 2020-06-15 | 2020-08-25 | 凯瑞环保科技股份有限公司 | Device and method for producing glycol diacrylate by using low-concentration ethylene glycol |
CN112608234A (en) * | 2020-12-30 | 2021-04-06 | 江苏盛叶欣化工新材料有限公司 | Method for producing high-content ethylene glycol diacetate and coproducing diethylene glycol diacetate |
Also Published As
Publication number | Publication date |
---|---|
CN110423197B (en) | 2023-11-14 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN110423197A (en) | A kind of device and method using low concentration ethylene glycol production glycol acetate | |
CN109369396A (en) | A kind of method that direct esterification prepares high-purity ethylene acetate | |
US11299450B2 (en) | System and process for co-producing dimethyl carbonate and ethylene glycol | |
CN109748805A (en) | The method of liquid ammonia process for caustic soda purification production isopropanolamine | |
CN101735182B (en) | Process for continuously producing succinic anhydride through hydrogenation of maleic anhydride | |
CN103274913A (en) | Method and device for producing methyl isobutyl ketone | |
CN106831315B (en) | Continuous production method of chloroethane | |
CN105111079A (en) | Method and device for separating acetic acid sec-butyl ester and sec-butyl alcohol | |
CN109134217B (en) | Oxidation device and oxidation process improvement method in cyclohexanone production process by cyclohexane oxidation method | |
CN108002995A (en) | A kind of method and its equipment of acetone two-step method synthesizing methyl isobutyl ketone | |
CN110483282B (en) | Device and method for producing high-concentration ethylene glycol diacetate | |
CN102718627B (en) | Preparation method of ethanol by adding hydrogen to ethyl acetate | |
CN107840808B (en) | Device for producing cyanoacetic acid ester and malonic acid ester by continuous reaction rectification and production process thereof | |
TW202005950A (en) | Integrated systems and processes for chemical production | |
CN210825997U (en) | Device for producing ethylene glycol diacetate by using low-concentration ethylene glycol | |
CN115531901A (en) | Reactor for synthesizing polymethoxy dimethyl ether by taking dimer as main raw material | |
CN109956845A (en) | A kind of propylene polymerization prepares the process of nonene | |
CN212335079U (en) | Production process device for synthesizing methyl methacrylate by methyl acetate and formaldehyde | |
CN211170522U (en) | Device for producing high-concentration ethylene glycol diacetate | |
CN103497130A (en) | Preparation method of D,L-2-hydroxy-4-methylthio butyric ester | |
CN209810143U (en) | Low boiling point alcohol continuous esterification reaction rectification system | |
CN112279783B (en) | Method for preparing 3-hydroxypropionitrile under supercritical condition | |
CN109369386A (en) | A kind of catalytic distillation prepares the devices and methods therefor of methyl formate | |
CN1332925C (en) | New technique for synthesizing isoamyl acetate | |
CN110818565A (en) | Device and process for preparing dimethyl carbonate by ester exchange method |
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 | ||
GR01 | Patent grant | ||
GR01 | Patent grant |