CN102060690A - 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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- CN102060690A CN102060690A CN 201110003631 CN201110003631A CN102060690A CN 102060690 A CN102060690 A CN 102060690A CN 201110003631 CN201110003631 CN 201110003631 CN 201110003631 A CN201110003631 A CN 201110003631A CN 102060690 A CN102060690 A CN 102060690A
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- underpressure distillation
- oxoethanoic acid
- phlegma
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Abstract
A glyoxylic acid refining and purifying method includes the following step 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 glyoxylic acid reaches 85 to 90 percent, 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 more and more higher to the technical requirements of oxoethanoic acid product.
In the prior art, the refining purification of oxoethanoic acid mainly is to remove the by product that produces in oxalic acid, oxalic dialdehyde and the reaction process from the thick product of oxoethanoic acid.Its process adopts ion-exchange and concentrated, 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 processing method very complicated, product yield is low, the equipment therefor complex structure, the product chloride ion content height after especially making with extra care, 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 of the present 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 ℃, opening vacuum and carry out underpressure distillation, underpressure distillation device internal pressure is controlled at 10-86kPa, progressively heat up, 2-8 ℃ of per minute 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 that contained oxoethanoic acid weight reaches 85-90% in the raw material, stop distillation, the phlegma that goes out with deionized water dilution second distillation obtains the oxoethanoic acid that content is 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, enters second stage underpressure distillation as the raw material of second stage underpressure distillation.
Above-mentioned oxoethanoic acid process for refining and purifying, in the described first step underpressure distillation, container inner pressure is controlled at 20-60kPa, 2-4 ℃ of per minute intensification, up to 85 ℃, constant temperature underpressure distillation 1 hour through condenser (2) condensation, is collected phlegma with distillate, finishes distillation.
Above-mentioned oxoethanoic acid process for refining and purifying, in the underpressure distillation of the described second stage, controlled temperature 180-200 ℃, container inner pressure is controlled at 20-60kPa, and weight reaches that contained oxoethanoic acid weight reaches at 90% o'clock 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, condenser and vacuum, and the top cover portion of described first step underpressure distillation device is provided with raw material and adds system, also also is communicated with a vacuum; Described condenser 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 described second stage underpressure distillation device is provided with products export; Described raw material adding system is storage tank and liquid-inlet pipe, and storage tank is communicated with the underpressure distillation device by 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, condenser; 3, second stage underpressure distillation device; 4, vacuum; 5, storage tank.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1
The refining device of purifying of oxoethanoic acid is 10 liters underpressure distillation still 1,3 by the two-stage volume, condenser 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 by liquid-inlet pipe; Underpressure distillation device 1 connects vacuum 4, and connects condenser 2 by drain pipe; Condenser 2 connects underpressure distillation device 3 by 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 company limited is produced is that 30% thick oxoethanoic acid raw material 50kg joins in the underpressure distillation still 1 through preserving jar 5, when being heated to 40 ℃, open vacuum 4 and carry out underpressure distillation, the container inner control is at 20kPa, progressively heat up, per minute heats up 2 ℃, up to 82 ℃, constant temperature underpressure distillation 1 hour through condenser 2 condensations, is collected phlegma with distillate, 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, reclaim the liquid total amount and reach 88% promptly during 13.2 kg of contained oxoethanoic acid weight in the raw material up to recording, stop 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%.
Embodiment 2
The refining device of purifying of oxoethanoic acid is 2000 milliliters four-hole glass reaction bottle 1,3 by the two-stage volume, condenser 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 by liquid-inlet pipe; Four-hole glass reaction bottle 1 connects vacuum 4, and connects condenser 2 by drain pipe; Condenser 2 connects four-hole glass reaction bottle 3 by 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 company limited is produced is that 40% thick oxoethanoic acid raw material 1000g joins in the four-hole glass reaction bottle 1 through preserving jar 5, when being heated to 40 ℃, open vacuum 4 and carry out underpressure distillation, the container inner control is at 60kPa, progressively heat up, per minute heats up 8 ℃, up to 87 ℃, constant temperature underpressure distillation 1 hour through condenser 2 condensations, is collected phlegma with distillate, 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, stop 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%.
Embodiment 3
The refining device of purifying of oxoethanoic acid is 1000 milliliters four-hole glass reaction bottle 1,3 by the two-stage volume, condenser 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 by liquid-inlet pipe; Four-hole glass reaction bottle 1 connects vacuum 4, and connects condenser 2 by drain pipe; Condenser 2 connects four-hole glass reaction bottle 3 by 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 company limited is produced is that 36% thick oxoethanoic acid raw material 600g joins in the four-hole glass reaction bottle 1 through preserving jar 5, when being heated to 40 ℃, open vacuum 4 and carry out underpressure distillation, the container inner control is at 40kPa, progressively heat up, per minute heats up 3 ℃, up to 85 ℃, constant temperature underpressure distillation 1 hour through condenser 2 condensations, is collected phlegma with distillate, 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, stop 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%.
Embodiment 4
The refining device of purifying of oxoethanoic acid is 500 liters underpressure distillation still 1,3 by the two-stage volume, condenser 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 by liquid-inlet pipe; Underpressure distillation device 1 connects vacuum 4, and connects condenser 2 by drain pipe; Condenser 2 connects underpressure distillation device 3 by 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 company limited is produced is that 35% thick oxoethanoic acid raw material 1000kg joins in the underpressure distillation still 1 through preserving jar 5, when being heated to 40 ℃, open vacuum 4 and carry out underpressure distillation, the container inner control is at 80kPa, progressively heat up, per minute heats up 5 ℃, up to 86 ℃, constant temperature underpressure distillation 1 hour through condenser 2 condensations, is collected phlegma with distillate, 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, stop 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%.
Embodiment 5
The refining device of purifying of oxoethanoic acid is 300 liters underpressure distillation still 1,3 by the two-stage volume, condenser 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 by liquid-inlet pipe; Underpressure distillation device 1 connects vacuum 4, and connects condenser 2 by drain pipe; Condenser 2 connects underpressure distillation device 3 by 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 company limited is produced is that 40% thick oxoethanoic acid raw material 600kg joins in the underpressure distillation still 1 through preserving jar 5, when being heated to 40 ℃, open vacuum 4 and carry out underpressure distillation, the container inner control is at 40kPa, progressively heat up, per minute heats up 3 ℃, up to 85 ℃, constant temperature underpressure distillation 1 hour through condenser 2 condensations, is collected phlegma with distillate, 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, stop 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), when being heated to 40 ℃, open vacuum (4) and carry out underpressure distillation, underpressure distillation device internal pressure is controlled at 10-86kPa, progressively heats up, 2-8 ℃ of per minute intensification, up to 82-87 ℃, constant temperature underpressure distillation 1 hour, with distillate through condenser (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 that contained oxoethanoic acid weight reaches 85-90% in the raw material, stop distillation, the phlegma that goes out with deionized water dilution second distillation obtains the oxoethanoic acid that content is 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, again phlegma and washing fluid are merged and obtain primary solution, enter 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, it is characterized in that, in the described first step underpressure distillation, container inner pressure is controlled at 20-60kPa, and 2-4 ℃ of per minute intensification is up to 85 ℃, constant temperature underpressure distillation 1 hour, distillate through condenser (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 described second stage, controlled temperature 180-200 ℃, container inner pressure is controlled at 20-60kPa, and weight reaches that contained oxoethanoic acid weight reaches at 90% o'clock 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), condenser (2) and vacuum (4), and the top cover portion of described first step underpressure distillation device (1) is provided with raw material and adds system, also also is communicated with a vacuum (4); Described condenser (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 described second stage underpressure distillation device (3) is provided with products export; Described raw material adding system is storage tank (5) and liquid-inlet pipe, and storage tank (5) is communicated with the underpressure distillation device by 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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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100036315A CN102060690B (en) | 2011-01-10 | 2011-01-10 | Glyoxylic acid refining and purifying method and device thereof |
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| Publication Number | Publication Date |
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| CN102060690A true CN102060690A (en) | 2011-05-18 |
| CN102060690B CN102060690B (en) | 2012-02-01 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110575677A (en) * | 2019-09-24 | 2019-12-17 | 成都理工大学 | Vacuum distillation device |
| WO2022258732A1 (en) | 2021-06-09 | 2022-12-15 | Avantium Knowledge Centre B.V. | Process and system for the recovery of glyoxylic acid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3872166A (en) * | 1972-07-01 | 1975-03-18 | Hermann Spaenig | Improvement in the recovery of glyoxylic acid |
| JPH11335320A (en) * | 1998-05-19 | 1999-12-07 | Nippon Shokubai Co Ltd | Production of alfa-oxocarboxylic acid |
-
2011
- 2011-01-10 CN CN2011100036315A patent/CN102060690B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3872166A (en) * | 1972-07-01 | 1975-03-18 | Hermann Spaenig | Improvement in the recovery of glyoxylic acid |
| JPH11335320A (en) * | 1998-05-19 | 1999-12-07 | Nippon Shokubai Co Ltd | Production of alfa-oxocarboxylic acid |
Non-Patent Citations (1)
| Title |
|---|
| 《化学世界》 2004 崔志敏 乙醛酸合成的研究 478-480 1-5 , 第5期 2 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110575677A (en) * | 2019-09-24 | 2019-12-17 | 成都理工大学 | Vacuum distillation device |
| CN110575677B (en) * | 2019-09-24 | 2021-08-03 | 成都理工大学 | Vacuum distillation device |
| WO2022258732A1 (en) | 2021-06-09 | 2022-12-15 | Avantium Knowledge Centre B.V. | Process and system for the recovery of glyoxylic acid |
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| Publication number | Publication date |
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| CN102060690B (en) | 2012-02-01 |
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