CN102826956A - Method for separating methyl propionate-methanol-water system by integration of salt-effect extraction and rectification - Google Patents
Method for separating methyl propionate-methanol-water system by integration of salt-effect extraction and rectification Download PDFInfo
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Abstract
The invention relates to a method for separating a methyl propionate-methanol-water system by integration of salt-effect extraction and rectification, which comprises the following steps: carrying out salt-effect extraction on a methyl propionate-methanol-water system by using saturated brine as an extractant; after the extraction separation, sending the water phase on the tower bottom of an extraction tower T1 to a methanol recovery tower T3, obtaining methanol of which the mass percent is higher than 99.98% from the T3 tower top and a salt concentrated solution from the T3 tower bottom, and returning the concentrated solution to the extraction tower T1 to be mixed with the extractant for cyclic use; and sending the organic phase from the tower top of the extraction tower T1 to a methyl propionate concentrating tower T2 for further methyl propionate concentration, obtaining a mixture of methyl propionate, methanol and water from the T2 tower top, sending the mixture to the extraction tower T2 to be mixed with the raw material solution for re-extraction, and obtaining methyl propionate of which the mass percent is higher than 99.97% from the T2 tower bottom, wherein the total yield is up to more than 89%. The invention has the advantages of simple technique, high separation efficiency, low production cost, environment friendliness, basically no discharge in the whole process, and the like.
Description
Technical field
The present invention relates to chemical separation technology, particularly a kind of salt is imitated extraction and the integrated method of separating methyl propionate-methanol-water system of rectifying.
Background technology
Methyl propionate can be used as the solvent of nitrocellulose, seasonings and spices, is used for also that nitro sprays paint, among the production process of coating.At present, the synthetic of methyl propionate mainly is catalyzer with the vitriol oil, made by propionic acid and methyl alcohol direct reaction, contains impurity such as free acid, alcohol and water in the reaction after product; Also contain a large amount of methyl propionates in the waste liquid that in the TEB 3K production process, produces.No matter be all to contain methyl propionate, methyl alcohol, water mixed solution in the waste liquid that produces in esterification or the TEB 3K production process.Methyl propionate is prone to form binary, ternary azeotrope with methyl alcohol, water in the above-mentioned mixing solutions, adopt traditional rectification method to be difficult to obtain highly purified methyl propionate, and energy consumption is higher.
The refining sodium hydrogencarbonate or the saturated solution of sodium carbonate of adopting usually of methyl propionate washed in the traditional industry, again with rectifying after yellow soda ash or the dried over sodium sulfate; Perhaps with the saturated sodium-chloride water solution washing, with distillation in the presence of Vanadium Pentoxide in FLAKES after the dried over anhydrous sodium carbonate, this process is complicated again, and equipment is perishable, and alkali and salt cycle process energy consumption are high, and a large amount of " three wastes " discharging is prone to form a series of environmental problems.
Chinese patent CN 102584525 A disclose a kind of with terepthaloyl moietie, 1; 2-Ucar 35, USP Kosher, methyl-phenoxide, toluene or chlorobenzene are extraction agent; Under normal pressure or reduced pressure; Adopt the method for batch extracting rectified separation of methanol-methyl propionate azeotropic mixture,, can obtain variant prodns such as methyl alcohol, methyl alcohol-methyl propionate, methyl propionate and methyl propionate-extraction agent in batches through control extractive distillation column tower top temperature and different reflux ratios.This patent is separation of methanol-methyl propionate azeotropic system effectively, but owing to adopt periodical operation, its process cost and energy consumption are higher, unstable product quality, and adopt toluene or chlorobenzene as extraction agent, its toxicity is bigger, is unfavorable for the workers with long time operation.
Summary of the invention
The objective of the invention is in order to overcome above deficiency; Provide a kind of technology simple, separation efficiency is high, is easy to obtain highly purified methyl propionate; And the process energy consumption reduces greatly; Save production cost, environmental friendliness, whole process realize the extraction of salt effect and the integrated method of separating methyl propionate-methanol-water system of rectifying of zero release basically.
The present invention realizes through following technical scheme: a kind of salt is imitated extraction and the integrated method of separating methyl propionate-methanol-water system of rectifying; May further comprise the steps: be extraction agent with the saturated brine; In extraction tower T1, methyl propionate-methanol-water system is carried out salt and imitate extraction; After the extracting and separating; Water at the bottom of the extraction tower T1 tower is delivered to methanol distillation column T3, and it is the methyl alcohol more than 99.98% that methanol distillation column T3 cat head obtains massfraction, and methanol distillation column T3 tower still obtains the liquid concentrator of salt; Recycle after again this liquid concentrator being turned back to extraction tower T1 and new extraction agent mixes; It is 97.57% methyl propionate that extraction tower T1 cat head organic phase obtains massfraction, this organic phase is delivered to methyl propionate upgrading tower T2 further carry dense methyl propionate, and it is 75.92% methyl propionate mixture that methyl propionate upgrading tower T2 cat head obtains massfraction; Again extract after again this methyl propionate mixture being delivered to extraction tower T1 and liquid stock is mixed, it is the methyl propionate more than 99.97% that methyl propionate upgrading tower T2 tower still obtains massfraction.
Further improvement of the present invention is, may further comprise the steps:
A, liquid stock get in the tower from the bottom of said extraction tower T1, with reverse contact of saturated brine that flows into extraction tower T1 inside from the liquid stock top, carry out counter-current extraction, and the mass ratio of liquid stock and saturated brine is 1～5:1;
The organic phase of B, said extraction tower T1 and the water residence time of leaving standstill in extraction tower T1 is 20 minutes, again organic phase and water is delivered to methyl propionate upgrading tower T2 and methanol distillation column T3 respectively, further reclaims methyl propionate and methyl alcohol;
C, said organic phase are after methyl propionate upgrading tower T2 handles; It is 75.92% methyl propionate mixture that methyl propionate upgrading tower T2 cat head obtains massfraction; Again extract after again this methyl propionate mixture being delivered to extraction tower T1 and liquid stock is mixed, it is the methyl propionate more than 99.97% that said methyl propionate upgrading tower T2 tower still obtains massfraction.
D, said water are after methanol distillation column T3 handles; It is the methyl alcohol more than 99.98% that said methanol distillation column T3 cat head obtains massfraction; Said methanol distillation column T3 tower still obtains the liquid concentrator of salt, recycles after again this liquid concentrator being turned back to extraction tower T1 and new extraction agent mixes.
Further improvement of the present invention is: said extraction agent is KCl or LiCl or NaCl or NH
4Cl or CaCl
2Or MgCl
2Or AlCl
3Or NaNO
3Or NH
4NO
3Or Na
2SO
4Or K
2SO
4Or MgSO
4Or Al
2(SO
4)
3Or Na
3PO
4Or NH
4H
2PO
4Or NaH
2PO
4Or K
2HPO
4Or (NH
4)
2HPO
4Or Na
2C
2O
4Or K
2C
2O
4Or CaC
2O
4Or Na
2CO
3Or K
2CO
3Or NaHSO
4Or KHSO
4Or KF or any two kinds or any two or more mixture.
Further improvement of the present invention is: the mass ratio of liquid stock described in the steps A and said saturated brine is 1:1.
Further improvement of the present invention is: when organic phase described in the step C was handled through methyl propionate upgrading tower T2, said methyl propionate upgrading tower T2 tower top temperature was 64.1～65.3 ℃, and tower still temperature is 79.7～80.6 ℃, and reflux ratio is 3～5.
Further improvement of the present invention is: when water described in the step D was handled through methanol distillation column T3, said methanol distillation column T3 tower top temperature was 64.5～65.3 ℃, and tower still temperature is 98.3～100.8 ℃, and reflux ratio is 1～3.
Further improvement of the present invention is: said extraction agent is NH
4H
2PO
4Or Al
2(SO
4)
3Or NaHSO
4Or any two kinds or any two or more mixture.
The present invention compared with prior art has the following advantages: can effectively separate methyl propionate-methanol-water system, separate back methyl propionate massfraction and reach more than 99.97%, total recovery reaches more than 89%; The methanol quality mark reaches more than 99.98%, and salts solution recycles after concentrating.The present invention not only technology is simple, and separation efficiency is high, is easy to obtain highly purified methyl propionate, and the process energy consumption reduces greatly, save production cost, and environmental friendliness, whole process realizes zero release basically.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention;
Label among the figure: 1. saturated brine, 2. liquid stock, 3. organic phase, 4. water, 5. 75.95% methyl propionate mixture, 6. methyl propionate, 7. methyl alcohol, 8. salt liquid concentrator, T1-extraction tower T1, T2-methyl propionate upgrading tower T2, T3-methanol distillation column T3.
Embodiment:
In order to deepen to understanding of the present invention, will combine embodiment and accompanying drawing that the present invention is made further detailed description below, this embodiment only is used to explain the present invention, does not constitute the qualification to protection domain of the present invention.
Show a kind of salt of the present invention like Fig. 1 and imitate extraction and the integrated embodiment of separating the method for methyl propionate-methanol-water system of rectifying; May further comprise the steps: 1. with saturated brine is extraction agent; In extraction tower T1, methyl propionate-methanol-water system is carried out salt and imitate extraction, after the extracting and separating, 4. water at the bottom of the extraction tower T1 tower is delivered to methanol distillation column T3; The T3 cat head obtain massfraction be more than 99.98% methyl alcohol 7.; 8. the liquid concentrator that T3 tower still obtains salt recycles after more 8. this liquid concentrator being turned back to extraction tower T1 and 1. new extraction agent mixes, and 3. extraction tower T1 cat head organic phase obtains massfraction is 97.57% methyl propionate; 3. this organic phase is delivered to methyl propionate upgrading tower T2 further carry dense methyl propionate; The T2 cat head obtain massfraction be 75.92% methyl propionate mixture 5., extract again after more 5. this mixture being delivered to extraction tower T1 and 2. liquid stock is mixed, T2 tower still obtain massfraction be more than 99.97% methyl propionate 6..
Further optimization step of the present invention comprises:
In 2. A, liquid stock get into tower from extraction tower T1 bottom, and 2. flow into inner 1. reverse contact of saturated brine of extraction tower T1 in the top from liquid stock, carry out counter-current extraction, 2. liquid stock is 1～5:1 with said saturated brine mass ratio 1.;
B, extraction tower T1 organic phase 3. with water 4. the residence time of leaving standstill in extraction tower T1 be 20 minutes, then 4. 3. this organic phase delivered to methyl propionate upgrading tower T2 and methanol distillation column T3 respectively with water, further reclaim methyl propionate and methyl alcohol;
C, organic phase are 3. after methyl propionate upgrading tower T2 handles; The T2 cat head obtain massfraction be 75.92% methyl propionate mixture 5.; Again extract after more 5. this mixture being delivered to extraction tower T1 and 2. liquid stock is mixed, T2 tower still obtain massfraction be more than 99.97% methyl propionate 6.;
D, said water are 4. after methanol distillation column T3 handles; Said T3 cat head obtain massfraction be more than 99.98% methyl alcohol 7.; 8. the liquid concentrator that said T3 tower still obtains salt recycles after more 8. this liquid concentrator being turned back to extraction tower T1 and 1. new extraction agent mixes.
Extraction agent described in the present invention is KCl or LiCl or NaCl or NH
4Cl or CaCl
2Or MgCl
2Or AlCl
3Or NaNO
3Or NH
4NO
3Or Na
2SO
4Or K
2SO
4Or MgSO
4Or Al
2(SO
4)
3Or Na
3PO
4Or NH
4H
2PO
4Or NaH
2PO
4Or K
2HPO
4Or (NH
4)
2HPO
4Or Na
2C
2O
4Or K
2C
2O
4Or CaC
2O
4Or Na
2CO
3Or K
2CO
3Or NaHSO
4Or KHSO
4Or KF, visible like table 1, salt can reduce the mutual solubility of system, makes that the massfraction of water and methyl alcohol lowers in the organic phase, reaches the purpose of dehydration and dealcoholysis, in conjunction with factors such as salt recovery difficulty or ease, preferably NH
4H
2PO
4Or Al
2(SO
4)
3Or NaHSO
4Be optimum extractant.
25 ℃ of following salts of table 1 are to the influence of system mutual solubility
Annotate: I, II, III are represented water, methyl alcohol, methyl propionate respectively.
The present invention adopts technology shown in Figure 1 and selected salt, can effectively separate methyl propionate-methanol-water system, separates back methyl propionate massfraction and reaches more than 99.97%, and total recovery reaches more than 89%; The methanol quality mark reaches more than 99.98%, and salts solution recycles after concentrating.
2. liquid stock described in the preferred steps A of the present invention is 1:1 with said saturated brine mass ratio 1., and 3. when methyl propionate upgrading tower T2 handled, the T2 tower top temperature was 64.1～65.3 ℃ to organic phase among the step C; Tower still temperature is 79.7～80.6 ℃; Reflux ratio is 3～5, and 4. when methanol distillation column T3 handled, the T3 tower top temperature was 64.5～65.3 ℃ to water among the step D; Tower still temperature is 98.3～100.8 ℃, and reflux ratio is 1～3.
Embodiment one: a kind of salt is imitated extraction and the integrated method of separating methyl propionate-methyl alcohol-aqueous systems of rectifying, and its concrete separation method may further comprise the steps:
Under A, the normal temperature, liquid stock is (contain methyl propionate 59.45%, methyl alcohol 25.35%, water 15.20% is massfraction) and NH 2.
4H
2PO
4Saturated brine mass rate 1. is 20 kg/h, and 2. liquid stock gets into from extraction tower T1 bottom, with the NH that flows into from extraction tower T1 top
4H
2PO
4The 1. reverse contact extracting and separating of saturated brine;
4. 3. B, organic phase all reach balance with water in every grade of extractor of multiple stage continuous adverse current extraction tower; Extract through 4 stage countercurrents; 3. 4. the residence time of leaving standstill in extraction tower T1 is 20 minutes to organic phase with water; Again 4. 3. organic phase delivered to methyl propionate upgrading tower T2 and methanol distillation column T3 respectively with water, further reclaim methyl propionate and methyl alcohol;
C, 3. organic phase is sent into methyl propionate regenerating column T2; The control inlet amount is 12.13kg/h, and the cat head load is 1.5kg/h, and control cat head and tower still temperature are respectively 65.3 ℃ and 79.7 ℃; Reflux ratio is 3; Number of theoretical plate is 30, and organic phase feed entrance point 3. is at the 15th column plate, the T2 cat head obtain massfraction be 75.92% methyl propionate mixture 5.; Again extract after more 5. this mixture being delivered to extraction tower T1 and 2. liquid stock is mixed, T2 tower still obtain massfraction be more than 99.97% methyl propionate 6.;
D, more 4. water is sent into methanol distillation column T3 through impeller pump, the control inlet amount is 27.87kg/h, and the cat head load is 19.5 kg/h; Control cat head, tower still temperature are respectively 64.5 ℃, 98.3 ℃, reflux ratio 1, number of theoretical plate 44; Water feed entrance point 4. is at the 25th block of column plate; 7. the T3 cat head obtains the methyl alcohol of massfraction more than 99.98%, and 8. the liquid concentrator that T3 tower still obtains salt recycles after more 8. this liquid concentrator being turned back to extraction tower T1 and 1. new extraction agent mixes.
The operating parameters of each tower and separating resulting are shown in table 2 and table 3 in the aforesaid method:
Table 2 tower operating parameters
The composition and the content (wt%) of each stream thigh in table 3 sepn process
Embodiment two: a kind of salt is imitated extraction and the integrated method of separating methyl propionate-methyl alcohol-aqueous systems of rectifying, and its concrete separation method may further comprise the steps:
Under A, the normal temperature, liquid stock is (contain methyl propionate 59.45%, methyl alcohol 25.35%, water 15.20% is massfraction) and Al 2.
2(SO
4)
3Saturated brine mass rate 1. is 20 kg/h, and 2. liquid stock gets into from extraction tower T1 bottom, with the Al that flows into from extraction tower T1 top
2(SO
4)
3The 1. reverse contact extracting and separating of saturated brine;
4. 3. B, organic phase all reach balance with water in every grade of extractor of multiple stage continuous adverse current extraction tower; Extract through 4 stage countercurrents; 3. 4. the residence time of leaving standstill in extraction tower T1 is 20 minutes to organic phase with water; Again 4. 3. organic phase delivered to methyl propionate upgrading tower T2 and methanol distillation column T3 respectively with water, further reclaim methyl propionate and methyl alcohol;
C, 3. organic phase is sent into methyl propionate regenerating column T2; The control inlet amount is 12.13kg/h, and the cat head load is 1.5kg/h, and control cat head and tower still temperature are respectively 64.8 ℃ and 80.2 ℃; Reflux ratio is 3; Number of theoretical plate is 30, and organic phase feed entrance point 3. is at the 15th column plate, the T2 cat head obtain massfraction be 76.83% methyl propionate mixture 5.; Again extract after more 5. this mixture being delivered to extraction tower T1 and 2. liquid stock is mixed, T2 tower still obtain massfraction be more than 99.93% methyl propionate 6.;
D, more 4. water is sent into methanol distillation column T3 through impeller pump, the control inlet amount is 27.87kg/h, and the cat head load is 19.5 kg/h; Control cat head, tower still temperature are respectively 64.9 ℃, 98.7 ℃, reflux ratio 1, number of theoretical plate 44; Water feed entrance point 4. is at the 25th block of column plate; 7. the T3 cat head obtains the methyl alcohol of massfraction more than 99.86%, and 8. the liquid concentrator that T3 tower still obtains salt recycles after more 8. this liquid concentrator being turned back to extraction tower T1 and 1. new extraction agent mixes.
Embodiment three: a kind of salt is imitated extraction and the integrated method of separating methyl propionate-methyl alcohol-aqueous systems of rectifying, and its concrete separation method may further comprise the steps:
Under A, the normal temperature, liquid stock is (contain methyl propionate 59.45%, methyl alcohol 25.35%, water 15.20% is massfraction) and NaHSO 2.
4Saturated brine mass rate 1. is 20 kg/h, and 2. liquid stock gets into from extraction tower T1 bottom, with the NaHSO that flows into from extraction tower T1 top
4The 1. reverse contact extracting and separating of saturated brine;
4. 3. B, organic phase all reach balance with water in every grade of extractor of multiple stage continuous adverse current extraction tower; Extract through 4 stage countercurrents; 3. 4. the residence time of leaving standstill in extraction tower T1 is 20 minutes to organic phase with water; Again 4. 3. organic phase delivered to methyl propionate upgrading tower T2 and methanol distillation column T3 respectively with water, further reclaim methyl propionate and methyl alcohol.
C, 3. organic phase is sent into methyl propionate regenerating column T2, the control inlet amount is 12.13kg/h, and the cat head load is 1.5kg/h; Control cat head and tower still temperature are respectively 65.1 ℃ and 79.8.2 ℃; Reflux ratio is 3, and number of theoretical plate is 30, and organic phase feed entrance point 3. is at the 15th column plate; The T2 cat head obtain massfraction be 76.83% methyl propionate mixture 5., extract again after more 5. this mixture being delivered to extraction tower T1 and 2. liquid stock is mixed; T2 tower still obtain massfraction be more than 99.87% methyl propionate 6..
D, more 4. water is sent into methanol distillation column T3 through impeller pump, the control inlet amount is 27.87kg/h, and the cat head load is 19.5 kg/h; Control cat head, tower still temperature are respectively 65.1 ℃, 99.6 ℃, reflux ratio 1, number of theoretical plate 44; Water feed entrance point 4. is at the 25th block of column plate; 7. the T3 cat head obtains the methyl alcohol of massfraction more than 99.91%, and 8. the liquid concentrator that T3 tower still obtains salt recycles after more 8. this liquid concentrator being turned back to extraction tower T1 and 1. new extraction agent mixes.
The present invention is through technology as shown in Figure 1 and selected salt, and salt can carry out two or more arbitrary combination, satisfies the actual treatment requirement; Perhaps to there being related parameter to adjust or implement corresponding conversion; Also can amplify accordingly in proportion, can effectively separate methyl propionate-methanol-water system according to the size of liquid stock treatment capacity; Separate back methyl propionate massfraction and reach more than 99.97%, total recovery reaches more than 89%; The methanol quality mark reaches more than 99.98%, and salts solution recycles after concentrating.The present invention not only technology is simple, and separation efficiency is high, is easy to obtain highly purified methyl propionate, and the process energy consumption reduces greatly, save production cost, and environmental friendliness, whole process realizes zero release basically.
Claims (7)
1. a salt is imitated extraction and the integrated method of separating methyl propionate-methanol-water system of rectifying; It is characterized in that; May further comprise the steps: be extraction agent with the saturated brine; In extraction tower T1, methyl propionate-methanol-water system is carried out salt and imitate extraction, after the extracting and separating, water at the bottom of the extraction tower T1 tower is delivered to methanol distillation column T3; It is the methyl alcohol more than 99.98% that said methanol distillation column T3 cat head obtains massfraction; Methanol distillation column T3 tower still obtains the liquid concentrator of salt, recycles after again this liquid concentrator being turned back to extraction tower T1 and new extraction agent mixes, and it is 97.57% methyl propionate that extraction tower T1 cat head organic phase obtains massfraction; This organic phase is delivered to methyl propionate upgrading tower T2 further carry dense methyl propionate; It is 75.92% methyl propionate mixture that said methyl propionate upgrading tower T2 cat head obtains massfraction, extracts again after again this methyl propionate mixture being delivered to extraction tower T1 and liquid stock is mixed, and it is the methyl propionate more than 99.97% that said methyl propionate upgrading tower T2 tower still obtains massfraction.
2. imitate extraction and the integrated method of separating methyl propionate-methanol-water system of rectifying according to the said salt of claim 1, it is characterized in that, comprise following concrete steps:
A, liquid stock get in the tower from the bottom of said extraction tower T1, with reverse contact of saturated brine that flows into extraction tower T1 inside from the liquid stock top, carry out counter-current extraction, and the mass ratio of liquid stock and said saturated brine is 1～5:1;
The organic phase of B, said extraction tower T1 and the water residence time of leaving standstill in extraction tower T1 is 20 minutes, again organic phase and water is delivered to methyl propionate upgrading tower T2 and methanol distillation column T3 respectively, further reclaims methyl propionate and methyl alcohol;
C, said organic phase are after methyl propionate upgrading tower T2 handles; It is 75.92% methyl propionate mixture that methyl propionate upgrading tower T2 cat head obtains massfraction; Again extract after again this methyl propionate mixture being delivered to extraction tower T1 and liquid stock is mixed, it is the methyl propionate more than 99.97% that said methyl propionate upgrading tower T2 tower still obtains massfraction;
D, said water are after methanol distillation column T3 handles; It is the methyl alcohol more than 99.98% that said methanol distillation column T3 cat head obtains massfraction; Said methanol distillation column T3 tower still obtains the liquid concentrator of salt, recycles after again this liquid concentrator being turned back to extraction tower T1 and new extraction agent mixes.
3. imitate extraction and the integrated method of separating methyl propionate-methanol-water system of rectifying according to claim 1 or 2 said salt, it is characterized in that: said extraction agent is KCl or LiCl or NaCl or NH
4Cl or CaCl
2Or MgCl
2Or AlCl
3Or NaNO
3Or NH
4NO
3Or Na
2SO
4Or K
2SO
4Or MgSO
4Or Al
2(SO
4)
3Or Na
3PO
4Or NH
4H
2PO
4Or NaH
2PO
4Or K
2HPO
4Or (NH
4)
2HPO
4Or Na
2C
2O
4Or K
2C
2O
4Or CaC
2O
4Or Na
2CO
3Or K
2CO
3Or NaHSO
4Or KHSO
4Or KF or any two kinds or any two or more mixture.
4. imitate extraction and the integrated method of separating methyl propionate-methanol-water system of rectifying according to the said salt of claim 2, it is characterized in that: the mass ratio of liquid stock described in the steps A and said saturated brine is 1:1.
5. imitate extraction and the integrated method of separating methyl propionate-methanol-water system of rectifying according to the said salt of claim 2; It is characterized in that: when organic phase described in the step C is handled through methyl propionate upgrading tower T2; Said methyl propionate upgrading tower T2 tower top temperature is 64.1～65.3 ℃; Tower still temperature is 79.7～80.6 ℃, and reflux ratio is 3～5.
6. imitate extraction and the integrated method of separating methyl propionate-methanol-water system of rectifying according to the said salt of claim 2; It is characterized in that: when water described in the step D is handled through methanol distillation column T3; Said methanol distillation column T3 tower top temperature is 64.5～65.3 ℃; Tower still temperature is 98.3～100.8 ℃, and reflux ratio is 1～3.
7. imitate extraction and the integrated method of separating methyl propionate-methanol-water system of rectifying according to the said salt of claim 3, it is characterized in that: said extraction agent is NH
4H
2PO
4Or Al
2(SO
4)
3Or NaHSO
4Or any two kinds or any two or more mixture.
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| CN103073423A (en) * | 2013-01-16 | 2013-05-01 | 南通大学 | Method for separating methyl propionate-methanol-water system by using rectification integration technology |
| CN103553875A (en) * | 2013-10-23 | 2014-02-05 | 安徽佳先功能助剂股份有限公司 | Recycling method of by-product in beta-diketone production |
| CN105218293A (en) * | 2015-09-01 | 2016-01-06 | 烟台大学 | A kind of method of separation of methylbenzene and alcohol mixture and device |
| CN112374989A (en) * | 2020-11-25 | 2021-02-19 | 西南化工研究设计院有限公司 | Separation method of mixture containing formaldehyde and methanol |
| CN112409178A (en) * | 2020-11-25 | 2021-02-26 | 西南化工研究设计院有限公司 | Method for preparing methyl methacrylate by taking methyl acetate as raw material |
| CN114524569A (en) * | 2022-03-04 | 2022-05-24 | 贵州正业龙腾新材料开发有限公司 | Waste water treatment device and process for production of polysiloxane microspheres |
| CN114524569B (en) * | 2022-03-04 | 2023-12-22 | 贵州正业龙腾新材料开发有限公司 | Wastewater treatment device and process for polyorganosiloxane microsphere production |
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