CN102924275A - Refining method for alcoholysis waste liquid in PVA (polyvinyl alcohol) production and test device for same - Google Patents
Refining method for alcoholysis waste liquid in PVA (polyvinyl alcohol) production and test device for same Download PDFInfo
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- CN102924275A CN102924275A CN2012104883156A CN201210488315A CN102924275A CN 102924275 A CN102924275 A CN 102924275A CN 2012104883156 A CN2012104883156 A CN 2012104883156A CN 201210488315 A CN201210488315 A CN 201210488315A CN 102924275 A CN102924275 A CN 102924275A
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Abstract
The invention relates to a refining method for an alcoholysis waste liquid in PVA (polyvinyl alcohol) production and a test device for the refining method, wherein the process method is that under the action of a catalyst, an extraction reaction rectification method is adopted, and acetic acid is added as an extractant and a reactant for reacting methanol in the azeotrope of methyl acetate and methanol to generate methyl acetate. The method specifically comprises the following steps of: 1) conveying the measured azeotrope of methyl acetate and methanol from the middle-lower part of an extraction reaction rectification tower, conveying the measured and proportioned extractant, namely, the acetic acid solution, from the upper part of the extraction reaction rectification tower, obtaining the methyl acetate in a concentration of 99.5% on the tower top of the extraction reaction rectification tower, and obtaining the acetic acid solution containing a small amount of methyl acetate, methanol and water on the tower bottom; and 2) conveying the residue from the extraction reaction rectification tower in an extractant recovery tower, rectifying out methyl acetate and methanol on the tower top of the extractant recovery tower and returning the methyl acetate and the methanol into the alcoholysis liquid azeotropic rectification tower of a PVA system, obtaining an acetic acid aqueous solution on the tower bottom of the extractant recovery tower and returning the acetic acid aqueous solution into the acetic acid concentration tower of the PVA system.
Description
Technical field
The present invention relates to the purification techniques of the pure liquid waste solution of a kind of polyvinyl alcohol (PVA), be specifically related to pure liquid waste solution process for purification and testing apparatus thereof in a kind of PVA production, the ritalin purification techniques that especially adopts extracting rectifying and reactive distillation to combine.
Background technology
In polyvinyl alcohol (PVA) production process, the Vinyl Acetate Copolymer alcoholysis can produce a large amount of by-product methyl acetates when generating polyvinyl alcohol, and generally, whenever synthetic 1 ton of PVA obtains approximately 1.68 tons of ritalins simultaneously.Ritalin purity is not high in the alcohol liquid waste solution, contains more methyl alcohol, and wherein methanol content is generally 74wt%, and ritalin is 18wt%, also has a small amount of other impurity, and the value of directly utilizing is little, usually need to carry out Separation and Recovery.The alcohol liquid waste solution generally passes through first azeotropic distillation, obtains thick methyl alcohol at the bottom of the tower, cat head obtains ritalin and methanol azeotrope, then take water as extraction agent with method separating acetic acid methyl esters and the methyl alcohol of extracting rectifying.But ritalin and water form azeotrope, contain 3.0 ~ 8.0% water and a small amount of methyl alcohol in the ritalin that the extracting rectifying cat head obtains, and the ritalin quality is not high, and industrial value is still little.Therefore the method for PVA factory following adopted fixed bed or reactive distillation is that acetic acid and methyl alcohol reclaim respectively with methyl acetate hydrolysis mostly.Because hydrolysis reaction is reversible reaction, ritalin can not be realized complete hydrolysis, and obtaining product after the hydrolysis is the quaternary product, wherein still has the separation problem of methyl acetate and methanol, ritalin-water azeotrope.The energy consumption of whole PVA factory has 50% ~ 60% to be used for recycle section, and the required energy consumption of recovery of acetic acid methyl esters accounts for about 70% of recycle section energy consumption.As seen seek a kind of technique is simple, energy consumption is low ritalin process for purification to PVA factory important in inhibiting.
Ritalin is a kind of important solvent and Organic Chemicals, at the industrial quick-drying solvent that is commonly used for PAA-CN-CA, being used for paint, is the raw material of making dyestuff and medicine, also can be used for the manufacturing of leatheroid and spices and the extraction agent that is used as grease.That high-purity methyl acetate can be used for is acetic acid synthesized, aceticanhydride, methyl acrylate, vinyl acetate between to for plastic and ethanamide etc.The market value of high-purity methyl acetate is compared the low-purity ritalin and is exceeded 2 ~ 4 times.Therefore, produce highly purified ritalin and have larger economic benefit.
Summary of the invention
The object of the present invention is to provide pure liquid waste solution process for purification and testing apparatus thereof in a kind of PVA production, the method is the technology that a kind of extracting rectifying and reactive distillation combine, be mainly used in refining polyvinyl alcohol industry by-product methyl acetate, overcome the difficulty of ritalin and methyl alcohol, ritalin and water Azeotrope separation, ritalin purity reaches more than 99.5% after refining, realizes the by-product resource utilization.The present invention makes that ritalin purification techniques technique is simple, less investment, energy consumption are low.
One of technical scheme of the present invention is: pure liquid waste solution process for purification during a kind of PVA produces, it is characterized in that this processing method is under the effect of catalyzer, adopt the extractive reaction rectificating method, add acetic acid as extraction agent and reactant, the reaction of methyl alcohol in ritalin and the methanol azeotrope is generated ritalin, specifically comprise the steps:
1) ritalin of metering and methanol azeotrope enter from the middle and lower part of extractive reaction rectifying tower, the extraction agent acetum of metering proportion enters from the top of extractive reaction rectifying tower, cat head at the extractive reaction rectifying tower obtains concentration 99.5% above ritalin, and tower reactor is the acetum that contains a small amount of ritalin, methyl alcohol, water;
2) the still liquid from the extractive reaction rectifying tower enters the extraction agent recovery tower, distillate the alcoholysis liquid azeotropy rectification column that ritalin and methyl alcohol return the PVA system at the cat head of extraction agent recovery tower, the tower reactor of described extraction agent recovery tower obtains the acetic acid concentration tower that aqueous acetic acid returns the PVA system.
Further, above-mentioned extractive reaction rectifying tower comprises rectifying section, extraction section, reactive distillation section and stripping section; It is rectifying section that extractive reaction rectifying tower top to acetic acid adds entrance, and it is extraction section that acetic acid adds entrance to the topmost of catalyst filling, and the part that catalyst filling is housed is the reactive distillation section, and ritalin and methanol azeotrope add that entrance is following to be stripping section.
Further, acetic acid destroys the binary azeotrope of ritalin, the formation of methanol in the extraction section of extractive reaction rectifying tower, generates ritalin with methyl alcohol in the reactive distillation section reaction of extractive reaction rectifying tower simultaneously; Obtain highly purified ritalin through cat head after the rectifying section rectifying separation of extractive reaction rectifying tower; A small amount of ritalin, unreacted methyl alcohol, water and acetic acid are discharged from the tower reactor of extractive reaction rectifying tower.
Further, described catalyzer is storng-acid cation exchange resin.
Further, the solvent ratio of described extraction agent and raw material is 2 ~ 3, and the reflux ratio of extractive reaction rectifying tower is 2 ~ 3, and described raw material is ritalin and methanol azeotrope.
Further, described extraction agent temperature is 5 ~ 40 ℃.
Further, described extractive reaction rectifying tower theoretical stage is 20 ~ 40; Extraction agent recovery tower theoretical stage 15 ~ 30.
Further, the reflux ratio of described extraction agent recovery tower is 0.2 ~ 1.0.
To sum up sum up: processing condition of the present invention are: enter methanol content 15% ~ 20% in the raw material ritalin carbinol mixture of rectifying tower; 5 ~ 40 ℃ of extraction agent temperature; Catalyzer is storng-acid cation exchange resin; Rectifying tower reflux ratio 2 ~ 3; Extraction agent recovery tower reflux ratio 0.2 ~ 1.0.Under such condition, the rectifying tower methanol conversion is greater than 85%, and product ritalin purity is greater than 99.5%.
Two of technical scheme of the present invention is: the refining testing apparatus of pure liquid waste solution during a kind of PVA produces, comprise be used to the first feed storage tank of depositing acetum, be used for depositing the second feed storage tank and the extractive reaction rectifying tower of ritalin and methanol azeotrope, it is characterized in that: described the first feed storage tank is led to the ingress, middle and upper part of extractive reaction rectifying tower through the first fresh feed pump, described the second feed storage tank is led to the ingress, middle and lower part of extractive reaction rectifying tower through the second fresh feed pump, the middle part of described extractive reaction rectifying tower is provided with catalyst filling, described extractive reaction rectifying tower top upside is provided with condenser, described extractive reaction rectifying tower top subordinate side is disposed with magnetic valve, reflux ratio controller and splitter, one branch road of described splitter is back to the rectifying section of extractive reaction rectifying tower, and another branch road of described splitter leads to product storage tank; Still liquid in the tower reactor of described extractive reaction rectifying tower pumps to the still liquid storage tank through still liquid extraction pump, rectifying section and the stripping section of described extractive reaction rectifying tower are respectively arranged with temperature controller, described tower reactor is arranged in the thermostatic bath, is provided with in the described tower reactor for the thermometer of measuring the still liquid temp.
Principal feature of the present invention and beneficial effect are as follows:
1, from the ritalin of PVA alcoholysis workshop section and methanol azeotrope (containing a small amount of other impurity), wherein ritalin content about 82%, methanol content about 18%, enter from extractive reaction rectifying tower middle and lower part, acetum enters from extractive reaction rectifying tower middle and upper part as extraction agent, cat head obtains the high-purity methyl acetate product, and tower reactor is the acetum that contains a small amount of ritalin, methyl alcohol, water.Still liquid goes out organism ritalin, methyl alcohol through extraction agent recovery tower rectifying separation, returns the PVA system alcoholysis liquid azeotropy rectification column that boils, and still liquid is the extraction agent aqueous acetic acid, recycles after returning PVA system acetic acid concentration tower concentrate.
The present invention has at first utilized acetic acid that then first alcohol and water extracting and separating from azeotrope is out made acetic acid and methyl alcohol reaction generate ritalin by esterification, thereby make highly purified ritalin.
2, the theoretical stage of extractive reaction rectifying tower is 20 ~ 40, and the number of theoretical plate of extraction agent recovery tower is 15 ~ 30 grades and is advisable.
3, the still liquid of extractive reaction rectifying tower enters the extraction agent recovery tower from the middle and lower part, and cat head distillates ritalin and methyl alcohol, and tower reactor obtains acetum and returns PVA system acetic acid concentration tower and recycle after concentrate.
4, maximum characteristics of the present invention are that technical process is simple, and energy-conservation, product purity is high.
Description of drawings
Fig. 1 is process flow diagram of the present invention.
Label declaration: T-101 extractive reaction rectifying tower, T-102 extraction agent recovery tower; A represents acetum, and b represents the ritalin methanol azeotrope, and c represents the ritalin product, and d stream thigh enters pure liquid waste solution azeotropy rectification column, and e stream thigh enters PVA system acetic acid concentration tower.
Fig. 2 is the testing apparatus schematic diagram of extractive reaction rectifying tower.
Label declaration: 1 first feed storage tank, 2 first fresh feed pumps, 3 second fresh feed pumps, 4 second feed storage tank, 5 thermometers, 6 tower reactors, 7 thermostatic baths, 8 still liquid extraction pumps, 9 still liquid storage tanks, 10 product storage tanks, 11,12,13 temperature controllers, 14 stripping sections, 15 reactive distillation sections, 16 rectifying sections, 17 reflux ratio controllers, 18 splitters, 19 magnetic valves, 20 condensers.
Embodiment
By describing technology contents of the present invention, structural attitude in detail, being realized purpose and effect, below in conjunction with embodiment and cooperate accompanying drawing to give in detail explanation.
Pure liquid waste solution process for purification during a kind of PVA produces, this processing method is under the effect of catalyzer, adopts the extractive reaction rectificating method, adds acetic acid as extraction agent and reactant, the reaction of methyl alcohol in ritalin and the methanol azeotrope is generated ritalin, specifically comprise the steps:
1) ritalin of metering and methanol azeotrope enter from the middle and lower part of extractive reaction rectifying tower, the extraction agent acetum of metering proportion enters from the top of extractive reaction rectifying tower, cat head at the extractive reaction rectifying tower obtains concentration 99.5% above ritalin, and tower reactor is the acetum that contains a small amount of ritalin, methyl alcohol, water;
2) the still liquid from the extractive reaction rectifying tower enters the extraction agent recovery tower, distillate the alcoholysis liquid azeotropy rectification column that ritalin and methyl alcohol return the PVA system at the cat head of extraction agent recovery tower, the tower reactor of described extraction agent recovery tower obtains the acetic acid concentration tower that aqueous acetic acid returns the PVA system.
In the present embodiment, described extractive reaction rectifying tower comprises rectifying section, extraction section, reactive distillation section and stripping section; It is rectifying section that extractive reaction rectifying tower top to acetic acid adds entrance, and it is extraction section that acetic acid adds entrance to the topmost of catalyst filling, and the part that catalyst filling is housed is the reactive distillation section, and ritalin and methanol azeotrope add that entrance is following to be stripping section.Acetic acid destroys the binary azeotrope of ritalin, the formation of methanol in the extraction section of extractive reaction rectifying tower, generate ritalin with methyl alcohol in the reactive distillation section reaction of extractive reaction rectifying tower simultaneously; Obtain highly purified ritalin through cat head after the rectifying section rectifying separation of extractive reaction rectifying tower; A small amount of ritalin, unreacted methyl alcohol, water and acetic acid are discharged from the tower reactor of extractive reaction rectifying tower.
In the present embodiment, described catalyzer is storng-acid cation exchange resin.The solvent ratio of described extraction agent and raw material is 2 ~ 3, and the reflux ratio of extractive reaction rectifying tower is 2 ~ 3, and described raw material is ritalin and methanol azeotrope.Described extraction agent temperature is 5 ~ 40 ℃.Described extractive reaction rectifying tower theoretical stage is 20 ~ 40; Extraction agent recovery tower theoretical stage 15 ~ 30.The reflux ratio of described extraction agent recovery tower is 0.2 ~ 1.0.
The refining testing apparatus of pure liquid waste solution during a kind of PVA produces, this testing apparatus comprises be used to the first feed storage tank 1 of depositing acetum, be used for depositing the second feed storage tank 4 and the extractive reaction rectifying tower of ritalin and methanol azeotrope, described the first feed storage tank 1 is led to the ingress, middle and upper part of extractive reaction rectifying tower through the first fresh feed pump 2, described the second feed storage tank 4 is led to the ingress, middle and lower part of extractive reaction rectifying tower through the second fresh feed pump 3, the middle part of described extractive reaction rectifying tower is provided with catalyst filling, described extractive reaction rectifying tower top upside is provided with condenser 20, described extractive reaction rectifying tower top subordinate side is disposed with magnetic valve 19, reflux ratio controller 17 and splitter 18, one branch road of described splitter 18 is back to the rectifying section 16 of extractive reaction rectifying tower, and another branch road of described splitter 18 leads to product storage tank 10; Still liquid in the tower reactor 6 of described extractive reaction rectifying tower pumps to still liquid storage tank 9 through still liquid extraction pump 8, the rectifying section of described extractive reaction rectifying tower and stripping section are respectively arranged with temperature controller 13,11, described tower reactor 6 is arranged in the thermostatic bath 7, is provided with in the described tower reactor 6 for the thermometer 5 of measuring the still liquid temp.
[embodiment 1]
Ritalin purification techniques of the present invention as shown in Figure 2, raw material is the 81.70wt% ritalin, 17.8wt% methyl alcohol adds tower T-101 from the middle and lower part; Extraction agent is acetum, adds tower T-101 from the middle and upper part.Tower is pressed and is normal pressure, and service temperature is 25 ℃ of room temperatures, solvent ratio 2:1, and reflux ratio is 2.5,31 grades of the theoretical stages of tower.Cat head obtains the product ritalin.The composition of cat head and tower reactor sees Table 1, the transformation efficiency 96.14% of methyl alcohol.Still liquid enters from solvent recovery tower T-102 tower middle and lower part, and cat head distillates ritalin, first alcohol and water, and still liquid is acetum.
[embodiment 2]
Difference from Example 1 is that solvent ratio is 3:1 among the embodiment 2, and transformation efficiency is 91.77%.Experimental result sees Table 2.
The above only is embodiments of the invention; be not so limit claim of the present invention; every equivalent structure or equivalent flow process conversion that utilizes specification sheets of the present invention and accompanying drawing content to do; or directly or indirectly be used in other relevant technical fields, all in like manner be included in the scope of patent protection of the present invention.
Claims (9)
1. pure liquid waste solution process for purification during a PVA produces, it is characterized in that this processing method is under the effect of catalyzer, adopt the extractive reaction rectificating method, add acetic acid as extraction agent and reactant, the reaction of methyl alcohol in ritalin and the methanol azeotrope is generated ritalin, specifically comprise the steps:
1) ritalin of metering and methanol azeotrope enter from the middle and lower part of extractive reaction rectifying tower, the extraction agent acetum of metering proportion enters from the top of extractive reaction rectifying tower, cat head at the extractive reaction rectifying tower obtains concentration 99.5% above ritalin, and tower reactor is the acetum that contains a small amount of ritalin, methyl alcohol, water;
2) the still liquid from the extractive reaction rectifying tower enters the extraction agent recovery tower, distillate the alcoholysis liquid azeotropy rectification column that ritalin and methyl alcohol return the PVA system at the cat head of extraction agent recovery tower, the tower reactor of described extraction agent recovery tower obtains the acetic acid concentration tower that aqueous acetic acid returns the PVA system.
2. pure liquid waste solution process for purification during PVA according to claim 1 produces, it is characterized in that: described extractive reaction rectifying tower comprises rectifying section, extraction section, reactive distillation section and stripping section; It is rectifying section that extractive reaction rectifying tower top to acetic acid adds entrance, and it is extraction section that acetic acid adds entrance to the topmost of catalyst filling, and the part that catalyst filling is housed is the reactive distillation section, and ritalin and methanol azeotrope add that entrance is following to be stripping section.
3. pure liquid waste solution process for purification during PVA according to claim 2 produces, it is characterized in that: acetic acid destroys the binary azeotrope of ritalin, the formation of methanol in the extraction section of extractive reaction rectifying tower, generates ritalin with methyl alcohol in the reactive distillation section reaction of extractive reaction rectifying tower simultaneously; Obtain highly purified ritalin through cat head after the rectifying section rectifying separation of extractive reaction rectifying tower; A small amount of ritalin, unreacted methyl alcohol, water and acetic acid are discharged from the tower reactor of extractive reaction rectifying tower.
4. pure liquid waste solution process for purification during PVA according to claim 1 produces, it is characterized in that: described catalyzer is storng-acid cation exchange resin.
5. pure liquid waste solution process for purification during PVA according to claim 1 produces, it is characterized in that: the solvent ratio of described extraction agent and raw material is 2 ~ 3, and the reflux ratio of extractive reaction rectifying tower is 2 ~ 3, and described raw material is ritalin and methanol azeotrope.
6. pure liquid waste solution process for purification during described PVA produces according to claim 1, it is characterized in that: described extraction agent temperature is 5 ~ 40 ℃.
7. pure liquid waste solution process for purification during PVA according to claim 1 produces, it is characterized in that: described extractive reaction rectifying tower theoretical stage is 20 ~ 40; Extraction agent recovery tower theoretical stage 15 ~ 30.
8. pure liquid waste solution process for purification during PVA according to claim 1 produces, it is characterized in that: the reflux ratio of described extraction agent recovery tower is 0.2 ~ 1.0.
9. the refining testing apparatus of pure liquid waste solution during a PVA produces, comprise be used to the first feed storage tank of depositing acetum, be used for depositing the second feed storage tank and the extractive reaction rectifying tower of ritalin and methanol azeotrope, it is characterized in that: described the first feed storage tank is led to the ingress, middle and upper part of extractive reaction rectifying tower through the first fresh feed pump, described the second feed storage tank is led to the ingress, middle and lower part of extractive reaction rectifying tower through the second fresh feed pump, the middle part of described extractive reaction rectifying tower is provided with catalyst filling, described extractive reaction rectifying tower top upside is provided with condenser, described extractive reaction rectifying tower top subordinate side is disposed with magnetic valve, reflux ratio controller and splitter, one branch road of described splitter is back to the rectifying section of extractive reaction rectifying tower, and another branch road of described splitter leads to product storage tank; Still liquid in the tower reactor of described extractive reaction rectifying tower pumps to the still liquid storage tank through still liquid extraction pump, rectifying section and the stripping section of described extractive reaction rectifying tower are respectively arranged with temperature controller, described tower reactor is arranged in the thermostatic bath, is provided with in the described tower reactor for the thermometer of measuring the still liquid temp.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103360247A (en) * | 2013-07-23 | 2013-10-23 | 福州大学 | Purification method of by-product acetic acid methyl ester |
| CN109467497A (en) * | 2018-08-03 | 2019-03-15 | 内蒙古蒙维科技有限公司 | A kind of recovery process and device of polyvinyl alcohol alcohol hydrolysis mother liquor |
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| CN101898963A (en) * | 2010-05-10 | 2010-12-01 | 南京师范大学 | Method for separating methyl acetate-methanol-water by adopting extractive distillation separation method with two-solvent lateral feed |
| CN102757342A (en) * | 2012-07-19 | 2012-10-31 | 安徽皖维高新材料股份有限公司 | Method for purifying by-product methyl acetate generated during production of PVA (polyvinyl acetate) |
| CN102766044A (en) * | 2012-08-07 | 2012-11-07 | 天津凯赛特科技有限公司 | Reaction and rectification system and method for recycling acetic acid from diluted acetic acid solution |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101898963A (en) * | 2010-05-10 | 2010-12-01 | 南京师范大学 | Method for separating methyl acetate-methanol-water by adopting extractive distillation separation method with two-solvent lateral feed |
| CN102757342A (en) * | 2012-07-19 | 2012-10-31 | 安徽皖维高新材料股份有限公司 | Method for purifying by-product methyl acetate generated during production of PVA (polyvinyl acetate) |
| CN102766044A (en) * | 2012-08-07 | 2012-11-07 | 天津凯赛特科技有限公司 | Reaction and rectification system and method for recycling acetic acid from diluted acetic acid solution |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103360247A (en) * | 2013-07-23 | 2013-10-23 | 福州大学 | Purification method of by-product acetic acid methyl ester |
| CN109467497A (en) * | 2018-08-03 | 2019-03-15 | 内蒙古蒙维科技有限公司 | A kind of recovery process and device of polyvinyl alcohol alcohol hydrolysis mother liquor |
| CN109467497B (en) * | 2018-08-03 | 2023-11-10 | 内蒙古蒙维科技有限公司 | Recovery process and device for polyvinyl alcohol alcoholysis mother liquor |
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