CN102060690B - Glyoxylic acid refining and purifying method and device thereof - Google Patents
Glyoxylic acid refining and purifying method and device thereof Download PDFInfo
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- CN102060690B CN102060690B CN2011100036315A CN201110003631A CN102060690B CN 102060690 B CN102060690 B CN 102060690B CN 2011100036315 A CN2011100036315 A CN 2011100036315A CN 201110003631 A CN201110003631 A CN 201110003631A CN 102060690 B CN102060690 B CN 102060690B
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Abstract
The invention relates to a glyoxylic acid refining and purifying method that includes the following steps of: primary reduced pressure distillation: adding crude glyoxylic acid into a primary reduced pressure distiller and heating to 40 DEG C, then starting a vacuumizer for reduced pressure distillation, controlling the pressure inside the reduced pressure distiller is controlled within 10 to 86 kPa, gradually raising the temperature to 82 to 87 DEG C, carrying out constant-temperature reduced pressure distillation for 1 hour, condensing the distillate by a condenser and transferring to a secondary reduced pressure distiller to be heated continuously and subjected to reduced pressure distillation, controlling the temperature to be within 160 to 220 DEG C and the pressure inside the container to be within 10 to 80 kPa, when the content of reclaimed liquid reaches 85 to 90 percent of the content of glyoxylic acid, stopping distillation, and diluting the secondary distilled condensate with deionized water so as to obtain the glyoxylic acid with the content of 40 to 50 percent, namely, the glyoxylic acid product is obtained. The method and device provided by the invention are simple and practical, and easy and feasible, and solve the problem that the traditional device has complicated structure and is difficult to operate.
Description
Technical field
The present invention relates to a kind of process for refining and purifying and device thereof, relate in particular to a kind of refining purification of oxoethanoic acid, belong to chemical technology field.
Background technology
Oxoethanoic acid, English name: glyoxylic acid, chemical formula: CHOCOOH, molecular weight: 74.04.Oxoethanoic acid is a kind of Organic Chemicals, is mainly prepared by the oxalic dialdehyde nitric acid oxidation.Along with the deepen continuously exploitation and the widespread use of oxoethanoic acid product, also increasingly high to the technical requirements of oxoethanoic acid product.
In the prior art, the refining purification of oxoethanoic acid mainly is from the thick product of oxoethanoic acid, to remove the by product that produces in oxalic acid, oxalic dialdehyde and the reaction process.Its process adopts IX and concentrates, the crystalline process for refining; Remove mineral acid, salt and oxalic acid through ion exchange resin earlier; Then through concentrating under reduced pressure, low temperature crystallization technology; Oxoethanoic acid is crystallized out with the form of glyoxylic acid, thereby oxoethanoic acid and oxalic dialdehyde and other organic by-products are separated.But this process method very complicated, product yield is low, the equipment therefor complex structure, the product chloride ion content after especially making with extra care is high, and product colour is dark, and use is restricted.
Summary of the invention
Technical problem to be solved by this invention is that the defective that overcomes prior art provides a kind of oxoethanoic acid process for refining and purifying, and the oxoethanoic acid of this method gained should have characteristics such as chloride ion content is few, of light color, and use range is wide.
Another problem that need solve of the present invention provides the refining device of purifying of oxoethanoic acid, the characteristics simple and practical, that be easy to make that this device should have of realizing.
Technical problem according to the invention is realized by following technical scheme.
A kind of oxoethanoic acid process for refining and purifying, it carries out as follows:
A. one-level underpressure distillation: measure the content of oxoethanoic acid in the thick oxoethanoic acid raw material and it is joined in the first step underpressure distillation device, when being heated to 40 ℃, the open vacuum device carries out underpressure distillation; Underpressure distillation device internal pressure is controlled at 10-86kPa, progressively heats up 2-8 ℃ of PM intensification; Up to 82-87 ℃, constant temperature underpressure distillation 1 hour, with distillate through condenser condenses; Collect phlegma, finish distillation, get primary solution;
B. second depressurized is distilled: gained primary solution among the step a is moved into continues heating in the second stage underpressure distillation device and carry out underpressure distillation; Controlled temperature 160-220 ℃; Container inner pressure is controlled at 10-80kPa, up to recording when reclaiming liquid weight and reaching the 85-90% of contained oxoethanoic acid weight in the raw material, stops distillation; The phlegma that uses deionized water dilution second distillation to go out obtains the oxoethanoic acid of content as 40%-50%, promptly gets the oxoethanoic acid product.
Above-mentioned oxoethanoic acid process for refining and purifying, gained phlegma in step a holds the container of phlegma with deionized water rinsing, phlegma and washing fluid is merged to obtain primary solution again, gets into second stage underpressure distillation as the raw material of second stage underpressure distillation.
Above-mentioned oxoethanoic acid process for refining and purifying, in the said first step underpressure distillation, container inner pressure is controlled at 20-60kPa, 2-4 ℃ of PM intensification, up to 85 ℃, constant temperature underpressure distillation 1 hour through condensing surface (2) condensation, is collected phlegma with distillate, finishes distillation.
Above-mentioned oxoethanoic acid process for refining and purifying, in the underpressure distillation of the said second stage, controlled temperature 180-200 ℃, container inner pressure is controlled at 20-60kPa, records to reclaim liquid weight and reach 90% o'clock of contained oxoethanoic acid weight in the raw material, stops distillation.
A kind of oxoethanoic acid is made with extra care purifying plant, and it is made up of first step underpressure distillation device, second stage underpressure distillation device, condensing surface and vacuum, and the top cover portion of said first step underpressure distillation device is provided with raw material and adds system, also also is communicated with a vacuum; Said condensing surface one end is communicated with first step underpressure distillation device, and the other end is communicated with second stage underpressure distillation device; The bottom of said second stage underpressure distillation device is provided with products export; Said raw material adding system is storage tank and liquid-inlet pipe, and storage tank is communicated with the underpressure distillation device through liquid-inlet pipe.
The present invention is according to the physical property of oxoethanoic acid; Oxoethanoic acid is extracted the problem that effectively solved existing oxoethanoic acid process for refining and purifying very complicated, product yield is low, chloride ion content is high, product colour is dark, use is restricted by underpressure distillation in the thick oxoethanoic acid mixture.Characteristics such as that refining purifying plant of the present invention has is simple in structure, easy handling, the problem that solved the existing apparatus complex structure, is difficult to operate is suitable for the refining purification of thick oxoethanoic acid in the produces tartronic process unit.
Description of drawings
Fig. 1 is apparatus of the present invention structural representation.
Each label is among the figure: 1, first step underpressure distillation device; 2, condensing surface; 3, second stage underpressure distillation device; 4, vacuum; 5, storage tank.
Embodiment
Below in conjunction with embodiment the present invention is done further explain.
The refining device of purifying of oxoethanoic acid is 10 liters underpressure distillation still 1,3 by the two-stage volume, condensing surface 2, and vacuum 4, thick oxoethanoic acid mixture storage tank 5 is formed; Underpressure distillation device 1 is connected with thick oxoethanoic acid mixture storage tank 5 through liquid-inlet pipe; Underpressure distillation device 1 connects vacuum 4, and connects condensing surface 2 through drain pipe; Condensing surface 2 connects underpressure distillation device 3 through drain pipe; Underpressure distillation device 3 bottoms are provided with the condensation liquid outlet, the outlet of the promptly refining back oxoethanoic acid product of purifying.
A. one-level underpressure distillation: the oxoethanoic acid content that mulberry field, Huanghua chemical industry ltd is produced is that 30% thick oxoethanoic acid raw material 50kg joins in the underpressure distillation still 1 through preserving jar 5, and when being heated to 40 ℃, open vacuum device 4 carries out underpressure distillation; The container inner control progressively heats up at 20kPa, and PM heats up 2 ℃; Up to 82 ℃, constant temperature underpressure distillation 1 hour, with distillate through condensing surface 2 condensations; Collect phlegma, finish distillation, shift out the phlegma of recovery; Hold the container of phlegma again with deionized water rinsing, with phlegma and washing fluid merge solution;
B. step a gained solution is moved into and continue heating in the underpressure distillation still 3 and carry out underpressure distillation; 180 ℃ of controlled temperature; The container inner control is at 20kPa, reclaims the liquid total amount and reaches 88% promptly during 13.2 kg of contained oxoethanoic acid weight in the raw material up to recording, and stops distillation; With the phlegma that deionized water dilution second distillation goes out, making content is 50% oxoethanoic acid product.
Product detects through the Cangzhou City product quality supervision and testing institute, and the result is: oxoethanoic acid content is 50%, chloride ion content 7.4ppm, oxalic acid content 0.08%, oxalic dialdehyde 0.16%.
The refining device of purifying of oxoethanoic acid is 2000 milliliters four-hole glass reaction bottle 1,3 by the two-stage volume, condensing surface 2, and vacuum 4, thick oxoethanoic acid mixture storage tank 5 is formed; Four-hole glass reaction bottle 1 is connected with thick oxoethanoic acid mixture storage tank 5 through liquid-inlet pipe; Four-hole glass reaction bottle 1 connects vacuum 4, and connects condensing surface 2 through drain pipe; Condensing surface 2 connects four-hole glass reaction bottle 3 through drain pipe; Four-hole glass reaction bottle 3 bottoms are provided with the condensation liquid outlet, the outlet of the promptly refining back oxoethanoic acid product of purifying.
A. one-level underpressure distillation: the oxoethanoic acid content that mulberry field, Huanghua chemical industry ltd is produced is that 40% thick oxoethanoic acid raw material 1000g joins in the four-hole glass reaction bottle 1 through preserving jar 5, and when being heated to 40 ℃, open vacuum device 4 carries out underpressure distillation; The container inner control progressively heats up at 60kPa, and PM heats up 8 ℃; Up to 87 ℃, constant temperature underpressure distillation 1 hour, with distillate through condensing surface 2 condensations; Collect phlegma, finish distillation, shift out the phlegma of recovery; Hold the container of phlegma again with deionized water rinsing, with phlegma and washing fluid merge solution;
B. step a gained solution is moved into and continue heating in the four-hole glass reaction bottle 3 and carry out underpressure distillation; 200 ℃ of controlled temperature; The container inner control is at 60kPa, up to recording when reclaiming the liquid total amount and reaching 90% of contained oxoethanoic acid weight in the raw material and be 360g, stops distillation; With the condensate recovery liquid that deionized water dilution second distillation goes out, making content is 50% oxoethanoic acid product.
Product detects through the Cangzhou City product quality supervision and testing institute, and the result is: oxoethanoic acid content is 50%, chloride ion content 6.1ppm, oxalic acid content 0.06%, oxalic dialdehyde 0.12%.
The refining device of purifying of oxoethanoic acid is 1000 milliliters four-hole glass reaction bottle 1,3 by the two-stage volume, condensing surface 2, and vacuum 4, thick oxoethanoic acid mixture storage tank 5 is formed; Four-hole glass reaction bottle 1 is connected with thick oxoethanoic acid mixture storage tank 5 through liquid-inlet pipe; Four-hole glass reaction bottle 1 connects vacuum 4, and connects condensing surface 2 through drain pipe; Condensing surface 2 connects four-hole glass reaction bottle 3 through drain pipe; Four-hole glass reaction bottle 3 bottoms are provided with the condensation liquid outlet, the outlet of the promptly refining back oxoethanoic acid product of purifying.
A. one-level underpressure distillation: the oxoethanoic acid content that mulberry field, Huanghua chemical industry ltd is produced is that 36% thick oxoethanoic acid raw material 600g joins in the four-hole glass reaction bottle 1 through preserving jar 5, and when being heated to 40 ℃, open vacuum device 4 carries out underpressure distillation; The container inner control progressively heats up at 40kPa, and PM heats up 3 ℃; Up to 85 ℃, constant temperature underpressure distillation 1 hour, with distillate through condensing surface 2 condensations; Collect phlegma, finish distillation, shift out the phlegma of recovery; Hold the container of phlegma again with deionized water rinsing, with phlegma and washing fluid merge solution;
B. step a gained solution is moved into and continue heating in the four-hole glass reaction bottle 3 and carry out underpressure distillation; 190 ℃ of controlled temperature; The container inner control is at 40kPa, up to recording when reclaiming the liquid total amount and reaching 89% of contained oxoethanoic acid weight in the raw material and be 194g, stops distillation; With the condensate recovery liquid that deionized water dilution second distillation goes out, making content is 50% oxoethanoic acid product.
Product detects through the Cangzhou City product quality supervision and testing institute, and the result is: oxoethanoic acid content is 50%, chloride ion content 5.7ppm, oxalic acid content 0.04%, oxalic dialdehyde 0.09%.
The refining device of purifying of oxoethanoic acid is 500 liters underpressure distillation still 1,3 by the two-stage volume, condensing surface 2, and vacuum 4, thick oxoethanoic acid mixture storage tank 5 is formed; Underpressure distillation device 1 is connected with thick oxoethanoic acid mixture storage tank 5 through liquid-inlet pipe; Underpressure distillation device 1 connects vacuum 4, and connects condensing surface 2 through drain pipe; Condensing surface 2 connects underpressure distillation device 3 through drain pipe; Underpressure distillation device 3 bottoms are provided with the condensation liquid outlet, the outlet of the promptly refining back oxoethanoic acid product of purifying.
A. one-level underpressure distillation: the oxoethanoic acid content that mulberry field, Huanghua chemical industry ltd is produced is that 35% thick oxoethanoic acid raw material 1000kg joins in the underpressure distillation still 1 through preserving jar 5, and when being heated to 40 ℃, open vacuum device 4 carries out underpressure distillation; The container inner control progressively heats up at 80kPa, and PM heats up 5 ℃; Up to 86 ℃, constant temperature underpressure distillation 1 hour, with distillate through condensing surface 2 condensations; Collect phlegma, finish distillation, shift out the phlegma of recovery; Hold the container of phlegma again with deionized water rinsing, with phlegma and washing fluid merge solution;
B. step a gained solution is moved into and continue heating in the underpressure distillation still 3 and carry out underpressure distillation; 200 ℃ of controlled temperature; The container inner control is at 50kPa, up to recording when reclaiming the liquid total amount and reaching 87% of contained oxoethanoic acid weight in the raw material and be 304.5kg, stops distillation; With the phlegma that deionized water dilution second distillation goes out, making content is 40% oxoethanoic acid product.
Product detects through the Cangzhou City product quality supervision and testing institute, and the result is: oxoethanoic acid content is 40%, chloride ion content 8.2ppm, oxalic acid content 0.07%, oxalic dialdehyde 0.13%.
The refining device of purifying of oxoethanoic acid is 300 liters underpressure distillation still 1,3 by the two-stage volume, condensing surface 2, and vacuum 4, thick oxoethanoic acid mixture storage tank 5 is formed; Underpressure distillation device 1 is connected with thick oxoethanoic acid mixture storage tank 5 through liquid-inlet pipe; Underpressure distillation device 1 connects vacuum 4, and connects condensing surface 2 through drain pipe; Condensing surface 2 connects underpressure distillation device 3 through drain pipe; Underpressure distillation device 3 bottoms are provided with the condensation liquid outlet, the outlet of the promptly refining back oxoethanoic acid product of purifying.
A. one-level underpressure distillation: the oxoethanoic acid content that mulberry field, Huanghua chemical industry ltd is produced is that 40% thick oxoethanoic acid raw material 600kg joins in the underpressure distillation still 1 through preserving jar 5, and when being heated to 40 ℃, open vacuum device 4 carries out underpressure distillation; The container inner control progressively heats up at 40kPa, and PM heats up 3 ℃; Up to 85 ℃, constant temperature underpressure distillation 1 hour, with distillate through condensing surface 2 condensations; Collect phlegma, finish distillation, shift out the phlegma of recovery; Hold the container of phlegma again with deionized water rinsing, with phlegma and washing fluid merge solution;
B. step a gained solution is moved into and continue heating in the underpressure distillation still 3 and carry out underpressure distillation; 200 ℃ of controlled temperature; The container inner control is at 60kPa, up to recording when reclaiming the liquid total amount and reaching 85% of contained oxoethanoic acid weight in the raw material and be 204kg, stops distillation; With the phlegma that deionized water dilution second distillation goes out, making content is 50% oxoethanoic acid product.
Product detects through the Cangzhou City product quality supervision and testing institute, and the result is: oxoethanoic acid content is 50%, chloride ion content 8.7ppm, oxalic acid content 0.09%, oxalic dialdehyde 0.24%.
Claims (5)
1. an oxoethanoic acid process for refining and purifying is characterized in that, it carries out as follows:
A. one-level underpressure distillation: thick oxoethanoic acid raw material is joined in the first step underpressure distillation device (1), and when being heated to 40 ℃, open vacuum device (4) carries out underpressure distillation; Underpressure distillation device internal pressure is controlled at 10-86kPa, progressively heats up 2-8 ℃ of PM intensification; Up to 82-87 ℃, constant temperature underpressure distillation 1 hour, with distillate through condensing surface (2) condensation; Collect phlegma, get primary solution;
B. second depressurized distillation: gained primary solution among the step a is moved into the middle continuation heating of second stage underpressure distillation device (3) and carries out underpressure distillation; Controlled temperature 160-220 ℃; Container inner pressure is controlled at 10-80kPa, up to recording when reclaiming liquid weight and reaching the 85-90% of contained oxoethanoic acid weight in the raw material, stops distillation; The phlegma that uses deionized water dilution second distillation to go out obtains the oxoethanoic acid of content as 40%-50%, promptly gets the oxoethanoic acid product.
2. oxoethanoic acid process for refining and purifying according to claim 1; It is characterized in that; Gained phlegma in step a; Hold the container of phlegma with deionized water rinsing, phlegma and washing fluid are merged obtain primary solution again, get into second stage underpressure distillation as the raw material of second stage underpressure distillation.
3. oxoethanoic acid process for refining and purifying according to claim 2 is characterized in that, in the said first step underpressure distillation; Container inner pressure is controlled at 20-60kPa, and 2-4 ℃ of PM intensification is up to 85 ℃; Constant temperature underpressure distillation 1 hour; Distillate through condensing surface (2) condensation, is collected phlegma, finish distillation.
4. oxoethanoic acid process for refining and purifying according to claim 3 is characterized in that, in the underpressure distillation of the said second stage; Controlled temperature 180-200 ℃; Container inner pressure is controlled at 20-60kPa, and weight reaches 90% o'clock of contained oxoethanoic acid weight in the raw material, stops distillation.
5. an oxoethanoic acid is made with extra care purifying plant; It is characterized in that; It is made up of first step underpressure distillation device (1), second stage underpressure distillation device (3), condensing surface (2) and vacuum (4), and the top cover portion of said first step underpressure distillation device (1) is provided with raw material and adds system, also also is communicated with a vacuum (4); Said condensing surface (2) one ends are communicated with first step underpressure distillation device, and the other end is communicated with second stage underpressure distillation device; The bottom of said second stage underpressure distillation device (3) is provided with products export; Said raw material adding system is storage tank (5) and liquid-inlet pipe, and storage tank (5) is communicated with the underpressure distillation device through liquid-inlet pipe.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011100036315A CN102060690B (en) | 2011-01-10 | 2011-01-10 | Glyoxylic acid refining and purifying method and device thereof |
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| CN2011100036315A CN102060690B (en) | 2011-01-10 | 2011-01-10 | Glyoxylic acid refining and purifying method and device thereof |
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| CN102060690A CN102060690A (en) | 2011-05-18 |
| CN102060690B true CN102060690B (en) | 2012-02-01 |
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| CN102786410A (en) * | 2012-07-26 | 2012-11-21 | 湖北省宏源药业有限公司 | Treating method and apparatus for reaction solution produced in synthesis of glyoxalic acid through nitric acid oxidation of glyoxal |
| CN110575677B (en) * | 2019-09-24 | 2021-08-03 | 成都理工大学 | Vacuum distillation device |
| US20240270673A1 (en) | 2021-06-09 | 2024-08-15 | Avantium Knowledge Centre B.V. | Process and system for the recovery of glyoxylic acid |
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| DE2232352B2 (en) * | 1972-07-01 | 1976-12-23 | Basf Ag, 6700 Ludwigshafen | PROCESS FOR THE PRODUCTION OF GLYOXYLIC ACID OR YOUR SODIUM SALT |
| JPH11335320A (en) * | 1998-05-19 | 1999-12-07 | Nippon Shokubai Co Ltd | Production of alfa-oxocarboxylic acid |
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