CN105218314B - The method that double extractive distillation columns combine separating isopropanol, the tert-butyl alcohol and water mixed solution - Google Patents

The method that double extractive distillation columns combine separating isopropanol, the tert-butyl alcohol and water mixed solution Download PDF

Info

Publication number
CN105218314B
CN105218314B CN201510402310.0A CN201510402310A CN105218314B CN 105218314 B CN105218314 B CN 105218314B CN 201510402310 A CN201510402310 A CN 201510402310A CN 105218314 B CN105218314 B CN 105218314B
Authority
CN
China
Prior art keywords
tert
butyl alcohol
isopropanol
extractive distillation
water
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.)
Expired - Fee Related
Application number
CN201510402310.0A
Other languages
Chinese (zh)
Other versions
CN105218314A (en
Inventor
顾正桂
冯微
孙昊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanjing Normal University
Original Assignee
Nanjing Normal University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nanjing Normal University filed Critical Nanjing Normal University
Priority to CN201510402310.0A priority Critical patent/CN105218314B/en
Publication of CN105218314A publication Critical patent/CN105218314A/en
Application granted granted Critical
Publication of CN105218314B publication Critical patent/CN105218314B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • C07C29/84Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

A kind of pair of extractive distillation column combines separating tert-butanol, the technique of isopropyl alcohol and water, mixed solution initially with the ethylene glycol solution separation of extractive distillation isopropanol, the tert-butyl alcohol and water of composite extractant 10~15% calcium chloride, tower top obtains more than 98.8% isopropanol and tert-butyl alcohol mixed liquor, bottom of towe is aqueous composite extractant, processes double solventss through regenerator and recycles;The tert-butyl alcohol that first extracting rectifying column overhead obtains separates through the second extractive distillation column with isopropanol mixed liquor, extractant is the sulfolane solution containing 20~30% propylene glycol, tower top can get more than 96.5% isopropanol, bottom of towe obtains the extractant containing tert-butyl alcohol mixed liquor, process through the second solvent regeneration tower, tower top obtains more than 96.4% tert-butyl alcohol, and bottom of towe is extracted agent and recycles.The extraction and separation technology of the present invention only needs reextraction rectification, and separating technology is simple, and isopropanol and t butanol content all reach more than 96.0%.

Description

The method that double extractive distillation columns combine separating isopropanol, the tert-butyl alcohol and water mixed solution
Technical field
The present invention relates to a kind of method that isopropanol and tertiary butanol aqueous solution recycle is and in particular to a kind of double extraction is smart Evaporate the method that tower combines separating isopropanol, the tert-butyl alcohol and water mixed solution.
Background technology
Isopropanol and the tert-butyl alcohol are important source material and the solvents of pesticide, dyestuff, medicine and spice.Isopropanol is mainly used in making Dehydrant, and the raw material and molten of pesticide intermediate preparation are used as on medicine, cosmetics, plastics, spice, coating and electronics industry Agent;Additionally, the abluent etc. also as circuit board and electronic equipment manufacturing industry, tool has been widely used.The tert-butyl alcohol as raw material, Can be used as fuel additive for internal combustion engines (preventing carburetor) and antidetonator;Intermediate as organic synthesiss and the tertiary fourth of production The raw material for alkylation of based compound, can produce methyl methacrylate, tert-butyl phenol, tert-butylamine etc., for synthetic drug, perfume (or spice) Material;Tert-butyl alcohol dehydration can produce the isobutene. of purity 99.0~99.9%;Solvent as industrial detergent, medicine extraction Agent, insecticide, wax solvent, the solvent of cellulose esters, plastics and paint, be additionally operable to manufacture denatured alcohol, spice, fruit essence, Isobutene. etc..
In chemical industry, medicine and pesticide intermediate produce, widely used isopropanol and the tert-butyl alcohol are as solvent or raw material, raw The mixed solution of a certain amount of isopropanol, the tert-butyl alcohol and water can be produced, for isopropanol and water, the tert-butyl alcohol and water during product Separate, seen both at home and abroad and carried out separating using methods such as distillation with adding salts, extraction and absorption, but for isopropanol, the tert-butyl alcohol and water The mixed liquor that three components are constituted separates, and respectively obtains highly purified isopropanol and the tert-butyl alcohol, and the method being recycled is still Have no report.
Content of the invention
The method that the present invention will provide a kind of pair of extractive distillation column to combine separating tert-butanol, isopropyl alcohol and water, the method work Skill step is simple,
For achieving the above object, the present invention adopts the following technical scheme that:
A kind of pair of extractive distillation column combine separating tert-butanol, the mixed solution of isopropyl alcohol and water method it is characterised in that The method stated comprise the steps:
1) initially with the mixed solution of composite extractant first time separation of extractive distillation isopropanol, the tert-butyl alcohol and water, institute The composite extractant stated is the ethylene glycol solution of 10~15wt% calcium chloride, and raw material mixed solution divides through the first extractive distillation column From rear, the first extracting rectifying tower top obtains isopropanol and the tert-butyl alcohol mixed liquor of more than 98.0wt%, the first extracting rectifying bottom of towe Obtain aqueous composite extractant;
2) the aqueous composite extractant obtained by the first extracting rectifying bottom of towe is through the first solvent regeneration tower rectification process, and first Solvent regeneration tower bottom of towe obtains composite extractant and is back to the first extractive distillation column recycling, and the first solvent reclamation column overhead obtains To water deliver to sewage-treatment plant;
3) the second extraction delivered to by more than the 98.0wt% tert-butyl alcohol that the first extracting rectifying column overhead obtains and isopropanol mixed liquor Rectifying column is taken to separate, the extractant of employing is the sulfolane solution of 10~15wt% propylene glycol, the tert-butyl alcohol and isopropanol mixed liquor After the second extractive distillation column extracting rectifying, the second extracting rectifying column overhead obtains the isopropanol of more than 96.0%wt, and second The extractant containing the tert-butyl alcohol for the extractive distillation column bottom of towe extraction;
4) extractant containing the tert-butyl alcohol of the second extractive distillation column bottom of towe extraction is through the second solvent regeneration tower rectification process, and the Two solvent regeneration tower bottom of towes are extracted agent, are back to the second extractive distillation column and recycle, the second solvent reclamation column overhead obtains The tert-butyl alcohol to more than 96.0wt%.
The extraction and separation technology of the present invention only needs reextraction rectification, and separating technology is simple, separate the isopropanol obtaining and T butanol content all reaches more than 96.0wt%, and one time yield all reaches more than 94.0%.
In described method, the mixed solution of raw material isopropanol, the tert-butyl alcohol and water its common consist of, with percent mass Ratio meter, isopropanol, the tert-butyl alcohol and water are respectively 58~62%, 28~32% and 6~12%.
In described method, the first extracting rectifying column overhead temperatures (DEG C) are 82.3~82.7 DEG C, and column bottom temperature (DEG C) is 105.4~110.2 DEG C, reflux ratio is 2~3:1.
In described method, the second extracting rectifying column overhead temperatures (DEG C) are 82.4~83.1 DEG C, and column bottom temperature (DEG C) is 107.8~110.9 DEG C, reflux ratio is 2~3:1.
In described method, the first solvent reclamation column overhead temperatures (DEG C) are 79.5~83.4 DEG C, and column bottom temperature (DEG C) is 142.7~146.6 DEG C, reflux ratio is 2~3:1.
In described method, the second solvent reclamation column overhead temperatures (DEG C) are 82.4~83.2 DEG C, and column bottom temperature (DEG C) is 144.2~146.8 DEG C, reflux ratio is 2~3:1.
Recommend ground, in described method,
The number of theoretical plate of the first extractive distillation column is 50, and feedstock position is the 45th plate, and extractant feed position is the 5th Plate;
The number of theoretical plate of the second extractive distillation column is 65, and feedstock position is the 52nd plate, and extractant feed position is the 10 plates;
First solvent regeneration tower number of theoretical plate is 25, and feedstock position is the 11st plate;
Second solvent regeneration tower number of theoretical plate is 22, and feedstock position is the 10th plate.
Beneficial effect:The extractive distillation column of the present invention combines separating tert-butanol, the technique of isopropyl alcohol and water, and step is simple, Initially with the mixed solution of composite extractant separation of extractive distillation isopropanol, the tert-butyl alcohol and water, tower top obtains more than 98.0% Isopropanol and tert-butyl alcohol mixed liquor, bottom of towe is aqueous composite extractant, through regenerator process double solventss recycle;The The tert-butyl alcohol that one extracting rectifying column overhead obtains separates through the second extractive distillation column with isopropanol mixed liquor, the second extractive distillation column The isopropanol on top available more than 96.0%, bottom of towe is the extractant containing tert-butyl alcohol mixed liquor, processes through the second solvent regeneration tower, Tower top obtains more than 96.0% tert-butyl alcohol, and bottom of towe is extracted agent and recycles.The extraction and separation technology of the present invention only needs two Secondary extracting rectifying, separating technology is simple, and isopropanol and t butanol content all reach more than 96.0%, yield all reach 94.0% with On.
Describe the present invention with reference to specific embodiment.Protection scope of the present invention is not to be embodied as Mode is limited, but is defined in the claims.
Brief description
Fig. 1 is the process chart that double extracting rectifyings combine separating tert-butanol, isopropanol and water mixed solution;
Fig. 2 is the Experimental equipment of extractive distillation column.
Specific embodiment
Below by specific embodiment, technical solutions according to the invention are further described in detail, but are necessary Point out that following examples are served only for the description to content of the invention, do not constitute limiting the scope of the invention.
Double extracting rectifyings of the present invention combine process chart such as Fig. 1 of separating tert-butanol, isopropanol and water mixed solution, With reference to Fig. 2, wherein 1 is the first extractive distillation column to the experimental provision of extractive distillation column, and 2 is the first solvent regeneration tower, and 3 is the second extraction Take rectifying column, 4 is the second solvent regeneration tower, 5,6,7,8 is condenser, 9,10,11,12 is reboiler, and 13 is head tank, and 14 are Raw material pump, 15 is glass rotameter, and 16 is tower reactor sampler, and 17 is electric jacket, and 18 is tower reactor, and 19 is bottom temperature meter, 20 is solvent feed tank, and 21 is pump, and 22 is glass rotameter, and 23 is glass fibre cotton and chuck, and 24 is filler, and 25 is tower top Sampler, 26 is refluxing opening, and 27 is tower top temperature meter, and 28 is electromagnetic wand, and 29 is condenser.
The tert-butyl alcohol being provided using certain drugmaker, the mixed solution of isopropyl alcohol and water are raw material, through the analysis of HP chromatograph, Composition is shown in Table 2, and if not otherwise indicated, is related to composition in material composition and table 2, table 3 and is mass content in below describing. The raw material tert-butyl alcohol, the mixed liquor of isopropyl alcohol and water add the first extractive distillation column 1, are simultaneously introduced composite extractant (10~15% The ethylene glycol solution of calcium chloride), after first time separation of extractive distillation, the first extractive distillation column 1 tower top can get mixed liquor More than 98.0% isopropanol and tert-butyl alcohol mixed liquor, bottom of towe is aqueous composite extractant, at the first solvent regeneration tower 2 Reason, the first solvent regeneration tower 2 bottom of towe obtains compound extracting and recycles, and the first solvent regeneration tower 2 tower top obtains water and delivers to sewage Pond;More than 98.0% tert-butyl alcohol being obtained with first time extracting rectifying and isopropanol mixed liquor, as raw material, enter the second extraction essence Evaporate tower 3 to separate, be simultaneously introduced extractant (sulfolane solutions of 10~15% propylene glycol), separate through reextraction rectification, second Extractive distillation column 3 tower top can get more than 96.0% isopropanol, and bottom of towe is the extractant containing tert-butyl alcohol mixed liquor, molten through second Agent regenerator 4 is processed, and the second solvent regeneration tower 4 bottom of towe is extracted agent and recycles, and the second solvent regeneration tower 4 head tower obtains More than 96.0% tert-butyl alcohol.
Experiment is carried out at ambient pressure, and extractive distillation column tower internal diameter is 22mm, built-inType stainless steel helices, through with marking Quasi- system of determination, this height equivalent to one theoretical plate HETP=27mm.Tower reactor is heated with electric jacket, overhead product discharging and raw material, solvent, Charging is all measured with glass rotameter, overhead reflux electricity consumption magnet regula, tower reactor vacuum pumped, and bottom of towe effluent send To solvent regeneration tower, solvent processes Posterior circle through regenerator and uses.
Specifically, the inventive method step is as follows:
1) 1. the mixed solution of raw material isopropanol, the tert-butyl alcohol and water is delivered to the first extractive distillation column 1 and is separated, and is simultaneously introduced multiple Close extractant 2., 1. after the first extractive distillation column 1 separates, the first extractive distillation column 1 tower top can once obtain mixed solution More than 98.0% isopropanol and tert-butyl alcohol mixed liquor 3., the first extractive distillation column 1 bottom of towe be aqueous composite extractant 4.;
2) 4. the aqueous composite extractant that first time separation of extractive distillation obtains is processed through the first solvent regeneration tower 2, the One solvent regeneration tower 2 bottom of towe obtains composite extractant and 2. recycles, and 5. the first solvent regeneration tower 2 overhead water delivers to cesspool;
3) 3. more than 98.0% tert-butyl alcohol that the first extractive distillation column 1 tower top obtains and isopropanol mixed liquor deliver to the second extraction Take rectifying column 3 to separate, be simultaneously introduced extractant 7., 3. the tert-butyl alcohol and isopropanol mixed liquor separate through the second extractive distillation column 3 Afterwards, 6., the second extractive distillation column 3 bottom of towe is containing tertiary fourth to the isopropanol of the second extractive distillation column 3 tower top available more than 96.0% The extractant of alcohol mixed liquor is 8.;
4) extractant containing tert-butyl alcohol mixed liquor that first time separation of extractive distillation obtains 8. through the second solvent regeneration tower 4 at Reason, the second solvent regeneration tower 4 bottom of towe is extracted agent and 7. recycles, and the second solvent regeneration tower 4 tower top obtains more than 96.0% The tert-butyl alcohol 9..
The process conditions of above-mentioned separation process:Each tower temperature control, reflux ratio, feed entrance point and the number of plates in separation process It is shown in Table 1, separating resulting is shown in Table shown in 2 and table 3.
Table 1 separation of extractive distillation process condition
2 pairs of extractive distillation columns of table combine separating tert-butanol-isopropanol-water mixed solution separating resulting
3 pairs of extractive distillation columns of table combine separating tert-butanol-isopropanol-water mixed solution separating resulting (Continued)
As shown in table 2 and table 3, this extraction and separation technology only needs reextraction rectification to separating resulting, and reflux ratio is 2~3:1 Left and right, separating technology is simple, and isopropanol and t butanol content all reach more than 96.0%, and one time yield all reaches more than 94.0%.

Claims (6)

1. a kind of pair of extractive distillation column combines the method for separating tert-butanol, the mixed solution of isopropyl alcohol and water it is characterised in that institute The method stated comprises the steps:
1) initially with the mixed solution of composite extractant first time separation of extractive distillation isopropanol, the tert-butyl alcohol and water, described Composite extractant is the ethylene glycol solution of 10~15wt% calcium chloride, and raw material mixed solution separates through the first extractive distillation column Afterwards, the first extracting rectifying tower top obtains isopropanol and the tert-butyl alcohol mixed liquor of more than 98.0wt%, and the first extracting rectifying bottom of towe obtains To aqueous composite extractant;
2) the aqueous composite extractant obtained by the first extracting rectifying bottom of towe is through the first solvent regeneration tower rectification process, the first solvent Regenerator bottom of towe obtains composite extractant and is back to the first extractive distillation column recycling, and the first solvent reclamation column overhead obtains Water delivers to sewage-treatment plant;
3) the second extraction essence delivered to by more than the 98.0wt% tert-butyl alcohol that the first extracting rectifying column overhead obtains and isopropanol mixed liquor Evaporate tower to separate, the extractant of employing is the sulfolane solution of 10~15wt% propylene glycol, the tert-butyl alcohol and isopropanol mixed liquor pass through After second extractive distillation column extracting rectifying, the second extracting rectifying column overhead obtains the isopropanol of more than 96.0%wt, the second extraction The extractant containing the tert-butyl alcohol for the rectifying tower bottom extraction;
4), through the second solvent regeneration tower rectification process, second is molten for the extractant containing the tert-butyl alcohol of the second extractive distillation column bottom of towe extraction Agent regenerator bottom of towe is extracted agent, is back to the second extractive distillation column and recycles, the second solvent reclamation column overhead obtains The tert-butyl alcohol of more than 96.0wt%.
2. the method for separating tert-butanol according to claim 1, the mixed solution of isopropyl alcohol and water is it is characterised in that institute The consisting of of the mixed solution of isopropanol, the tert-butyl alcohol and water stated, by percentage to the quality, isopropanol, the tert-butyl alcohol and water are respectively For 58~62%, 28~32% and 6~12%.
3. the method for separating tert-butanol according to claim 1, the mixed solution of isopropyl alcohol and water is it is characterised in that institute In the method stated, the first extracting rectifying column overhead temperatures (DEG C) are 82.3~82.7 DEG C, column bottom temperature (DEG C) for 105.4~ 110.2 DEG C, reflux ratio is 2~3: 1.
4. the method for separating tert-butanol according to claim 1, the mixed solution of isopropyl alcohol and water is it is characterised in that institute In the method stated, the second extracting rectifying column overhead temperatures (DEG C) are 82.4~83.1 DEG C, column bottom temperature (DEG C) for 107.8~ 110.9 DEG C, reflux ratio is 2~3: 1.
5. the method for separating tert-butanol according to claim 1, the mixed solution of isopropyl alcohol and water is it is characterised in that institute In the method stated, the first solvent reclamation column overhead temperatures (DEG C) are 79.5~83.4 DEG C, column bottom temperature (DEG C) for 142.7~ 146.6 DEG C, reflux ratio is 2~3: 1.
6. the method for separating tert-butanol according to claim 1, the mixed solution of isopropyl alcohol and water is it is characterised in that institute In the method stated, the second solvent reclamation column overhead temperatures (DEG C) are 82.4~83.2 DEG C, column bottom temperature (DEG C) for 144.2~ 146.8 DEG C, reflux ratio is 2~3: 1.
CN201510402310.0A 2015-07-10 2015-07-10 The method that double extractive distillation columns combine separating isopropanol, the tert-butyl alcohol and water mixed solution Expired - Fee Related CN105218314B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510402310.0A CN105218314B (en) 2015-07-10 2015-07-10 The method that double extractive distillation columns combine separating isopropanol, the tert-butyl alcohol and water mixed solution

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510402310.0A CN105218314B (en) 2015-07-10 2015-07-10 The method that double extractive distillation columns combine separating isopropanol, the tert-butyl alcohol and water mixed solution

Publications (2)

Publication Number Publication Date
CN105218314A CN105218314A (en) 2016-01-06
CN105218314B true CN105218314B (en) 2017-03-08

Family

ID=54987660

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510402310.0A Expired - Fee Related CN105218314B (en) 2015-07-10 2015-07-10 The method that double extractive distillation columns combine separating isopropanol, the tert-butyl alcohol and water mixed solution

Country Status (1)

Country Link
CN (1) CN105218314B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108997087B (en) * 2018-08-21 2021-05-18 上海兖矿能源科技研发有限公司 Separation method of n-propanol and 2-butanol mixed solution

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
分隔壁共沸精馏塔分离叔丁醇水混合物的模拟研究;叶青;《天然气化工》;20091231;第34卷(第5期);17-20,23 *
异丙醇-水分离技术研究新进展;汪宝和等;《化学研究》;20070630;第18卷(第2期);103-106 *
间歇萃取精馏分离叔丁醇与水共沸物的研究;缪英等;《常州大学学报(自然科学版)》;20121231;第24卷(第4期);34-36 *

Also Published As

Publication number Publication date
CN105218314A (en) 2016-01-06

Similar Documents

Publication Publication Date Title
CN105001056A (en) Method for separating isobutyl alcohol and normal heptanes azeotropic system by using pressure swing distillation
CN107445817A (en) A kind of method with ion liquid abstraction rectifying acetone and methanol
CN103755559A (en) Method for separating ethyl acetate-isopropanol by ionic liquid extractive rectification
CN105175280A (en) Acetonitrile-tert-butanol azeotropic mixture continuous extraction rectification separation method
CN105272819A (en) Purification method of methanol containing ethyl acetate impurity
CN104447198B (en) Separation technology for preparation of isopropanol by acetone hydrogenation
CN104844433A (en) Method for separating acetone/DMF/water ternary system by rectifying through high- and low- pressure towers
CN105001055B (en) Based on mixed solvent as extractant isopropanol acetonitrile azeotropic mixture distillation and separation method
CN106008186A (en) Method for separating acetone, isopropanol and water mixed solution
CN105218314B (en) The method that double extractive distillation columns combine separating isopropanol, the tert-butyl alcohol and water mixed solution
CN103772185B (en) Device and method for removing moisture and heteroacids in acetic acid
CN104370693A (en) Separation method for batch extractive distillation of methanol-propyl formate azeotrope
CN106349107B (en) A kind of method and device of heterogeneous azeotropic rectification separating acetonitrile-triethylamine mixture
CN102531834A (en) System and process for recovering waste liquid in 1, 4-butanediol production process
CN105061146A (en) Batch distillation process for separating isopropanol-acetonitrile azeotrope through mixed extraction agent
CN106431880B (en) Novel variable-pressure rectification acetone, isopropyl ether object system method
CN204352584U (en) With the device that chlorination 1-(2-chloroethyl)-3-methylimidazole is extractant tert-butyl alcohol from water
CN105001053A (en) Isopropanol-propyl formate azeotrope rectification separation method based on mixed solvent as extracting agent
CN105646146A (en) Propyl alcohol-triethylamine azeotropic mixture extraction and rectification method
CN104383711B (en) It is the devices and methods therefor of extractant tert-butyl alcohol from water with chlorination 1-(2-chloroethyl)-3-methylimidazole
CN105037155A (en) Batch distillation process for separating tert-butyl alcohol-methyl propionate azeotrope by mixed extractant
CN105152926A (en) Distillation separation method for azeotrope of tert-butanol and methylpropionate by using mixed solvent as extractant
CN109704919A (en) Water-methanol-ethanol mixture extractive distillation separation method based on choline chloride eutectic solvent
CN104693005A (en) New process for separating methanol-propyl formate azeotrope through extractive distillation
CN204111623U (en) A kind of process unit of purifying for by product diisopropyl ether in Virahol production

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20170308

CF01 Termination of patent right due to non-payment of annual fee