CN111689910B - Method for removing impurity iodine in pyrazine compound - Google Patents
Method for removing impurity iodine in pyrazine compound Download PDFInfo
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- CN111689910B CN111689910B CN202010565609.9A CN202010565609A CN111689910B CN 111689910 B CN111689910 B CN 111689910B CN 202010565609 A CN202010565609 A CN 202010565609A CN 111689910 B CN111689910 B CN 111689910B
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- C07D241/00—Heterocyclic compounds containing 1,4-diazine or hydrogenated 1,4-diazine rings
- C07D241/02—Heterocyclic compounds containing 1,4-diazine or hydrogenated 1,4-diazine rings not condensed with other rings
- C07D241/10—Heterocyclic compounds containing 1,4-diazine or hydrogenated 1,4-diazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D241/12—Heterocyclic compounds containing 1,4-diazine or hydrogenated 1,4-diazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached to ring carbon atoms
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Abstract
The application relates to a method for removing impurity iodine in a pyrazine compound, which comprises the following steps: (a) forming a pyrazine compound solution containing impurity iodine; (b) adding silver carbonate powder into the pyrazine compound solution, and heating the pyrazine compound solution to enable the silver carbonate powder to react with impurity iodine in the pyrazine compound solution to form a mixed solution; (c) carrying out sedimentation treatment on the mixed solution; (d) and centrifuging the settled supernatant after the settlement is finished to obtain a pyrazine compound solution without impurity iodine. This application is through adding silver carbonate powder in the pyrazine compound solution that contains impurity iodine, makes impurity iodine and silver carbonate powder produce chemical reaction and generates other materials to clear away the impurity iodine in pyrazine compound solution, reach the purpose of impurity iodine in the quick removal pyrazine compound, and the haze that utilizes the light adjusting film of the pyrazine compound preparation that this application prepared reduces to about 5%, satisfies the haze demand of light adjusting film.
Description
Technical Field
The application relates to a pyrazine compound, in particular to a method for removing impurity iodine in the pyrazine compound.
Background
Pyrazine compounds are effective functional molecules which can be applied to intelligent light modulation films, and the integral appearance and functional effect of the film can be greatly influenced even if trace impurities exist in the intelligent light modulation films, so that the pyrazine compounds are imperative to iodine removal.
In the process of implementing the application, the applicant finds that the conventional method for removing impurity iodine in the pyrazine compound mainly comprises the steps of carrying out centrifugal treatment on a pyrazine compound solution for multiple times, then dispersing and dissolving by adopting a solvent, and removing the impurity iodine in the pyrazine compound, wherein the whole removing process is long in time consumption, and has high requirements on equipment.
Disclosure of Invention
The embodiment of the application provides a method for removing impurity iodine in a pyrazine compound, and solves the problems that the time consumption is long and the requirement on equipment is high in the existing removal process of impurity iodine in the pyrazine compound.
In order to solve the above technical problem, the present application is implemented as follows:
in a first aspect, a method for removing impurity iodine in a pyrazine compound is provided, which comprises the following steps:
(a) forming a pyrazine compound solution containing impurity iodine;
(b) adding silver carbonate powder into the pyrazine compound solution, and heating the pyrazine compound solution to enable the silver carbonate powder to react with impurity iodine in the pyrazine compound solution to form a mixed solution;
(c) carrying out sedimentation treatment on the mixed solution;
(d) and centrifuging the settled supernatant after the settlement is finished to obtain a pyrazine compound solution without impurity iodine.
In a first possible implementation manner of the first aspect, in the step (a), the impurity iodine-containing pyrazine compound is dissolved in isoamyl acetate to form an impurity iodine-containing pyrazine compound solution.
With reference to the first possible implementation manner of the first aspect, in a second possible implementation manner of the first aspect, the pyrazine compound containing iodine as an impurity and isoamyl acetate are placed in a three-neck flask, the three-neck flask is heated, and the pyrazine compound and the isoamyl acetate are stirred to dissolve the pyrazine compound in the isoamyl acetate.
With reference to the second possible implementation manner of the first aspect, in a third possible implementation manner of the first aspect, the manner of heating the three-necked flask is water bath heating, the water bath heating temperature is 70 degrees celsius, the speed of stirring the pyrazine compound and the isoamyl acetate is 300 revolutions per minute, and the dissolving time of the pyrazine compound is 8 hours.
In a fourth possible implementation manner of the first aspect, in the step (b), the temperature when the pyrazine compound solution is heated is 70 degrees celsius.
In a fifth possible implementation manner of the first aspect, in the step (b), the step of heating the pyrazine compound solution further includes the step of performing an iodine-containing test on the pyrazine compound solution.
With reference to the fifth possible implementation manner of the first aspect, in a sixth possible implementation manner of the first aspect, the method for iodine-containing testing comprises the following steps:
preparing a starch solution;
and adding part of the pyrazine compound solution into the starch solution, judging that iodine still exists in the pyrazine compound solution if the starch solution turns yellow, continuing heating the pyrazine compound solution, otherwise, judging that iodine does not exist in the pyrazine compound solution, and stopping heating the pyrazine compound solution.
In a seventh possible implementation manner of the first aspect, in the step (c), after the mixed solution is subjected to the sedimentation treatment, the method further includes the steps of discharging a sedimentation lower layer solution and collecting a sedimentation upper layer solution.
In an eighth possible implementation manner of the first aspect, in the step (d), when the sedimentation supernatant is subjected to the centrifugation treatment, the centrifugation speed is 4000rpm, and the centrifugation time is 60 minutes.
In a ninth possible implementation manner of the first aspect, in the step (d), after the sedimentation supernatant is subjected to a centrifugation process, a centrifugation supernatant after centrifugation of the sedimentation supernatant is collected, and the centrifugation supernatant is a pyrazine compound solution containing no impurity iodine.
Compared with the prior art, the application has the advantages that:
the method for removing impurity iodine in pyrazine compound comprises the steps of adding silver carbonate powder into pyrazine compound solution containing impurity iodine, enabling impurity iodine and silver carbonate powder to generate chemical reaction to generate other substances, removing impurity iodine in the pyrazine compound solution, achieving the purpose of quickly removing impurity iodine in the pyrazine compound, reducing the haze of a light modulation film prepared from the pyrazine compound to about 5%, and meeting the haze requirement of the light modulation film.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
fig. 1 is a schematic flow chart illustrating a process of removing iodine impurity from pyrazine compound according to an embodiment of the present disclosure.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some, but not all, embodiments of the present application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
In an embodiment of the present application, please refer to fig. 1, which is a schematic flow chart illustrating a process of removing iodine impurity from a pyrazine compound according to an embodiment of the present application. As shown in the figure, the method 1 for removing impurity iodine from pyrazine compound includes the following steps 101-104, wherein:
specifically, a pyrazine compound containing impurity iodine and isoamyl acetate are placed in a three-neck flask, the three-neck flask is heated in a water bath heating mode, the water bath heating temperature is set to be 70 ℃, the pyrazine compound and the isoamyl acetate are stirred at the same time, the stirring speed is 300rpm, the pyrazine compound is dissolved in the isoamyl acetate, and the dissolving time is 8 hours.
Specifically, a proper amount of silver carbonate powder is added into a three-neck flask, and the silver carbonate powder and impurity iodine in the pyrazine compound solution are subjected to chemical reaction to form silver iodide, and the silver iodide is precipitated to form a mixed solution. And simultaneously heating and stirring the pyrazine compound solution to promote the reaction of the silver carbonate powder and impurity iodine to rapidly proceed, wherein the heating temperature is 70 ℃.
Meanwhile, stirring is suspended after the heating and stirring are carried out for 4 hours, and part of the mixed solution is taken for carrying out iodine-containing test. Specifically, putting starch into boiling water, preparing a starch solution, adding an upper layer solution in the mixed solution into the starch solution, judging that iodine still exists in the mixed solution if the starch solution turns yellow, continuing to heat the mixed solution, otherwise, judging that iodine does not exist in the mixed solution, stopping adding the mixed solution, judging that iodine still exists in the mixed solution if the starch solution turns yellow, continuing to heat the mixed solution, otherwise, judging that iodine does not exist in the mixed solution, and stopping heating the mixed solution.
And step 103, settling treatment. And (5) performing sedimentation treatment on the mixed solution.
Specifically, after the mixed solution is judged to be free of iodine and the pyrazine compound solution is stopped heating, the mixed solution is transferred to a 5000ml separating funnel, is kept stand for 5 hours, then the sedimentation lower layer solution is discharged, and the sedimentation upper layer solution is collected.
And step 104, centrifuging. And centrifuging the settled supernatant after the settlement is finished to obtain a pyrazine compound solution without impurity iodine.
Specifically, the TDZ5-WS type centrifuge is used for carrying out centrifugal treatment on the obtained sedimentation supernatant, the set rotating speed in the centrifugal process is 4000rpm, the centrifugal time is 60min, after the centrifugal treatment, the centrifugal supernatant obtained after the sedimentation supernatant is centrifuged is collected, and the centrifugal supernatant is a pyrazine compound solution containing no impurity iodine, namely the required high-purity pyrazine compound solution.
The following will further illustrate the beneficial effects of the method for removing impurity iodine from pyrazine compounds of the present application with reference to specific examples and comparative examples.
Example 1
1. Taking 500g of pyrazine compound solution, 100g of silver carbonate powder and 2L of a three-mouth glass bottle;
2. mixing the two, putting into 70 ℃ water bath, and mechanically stirring for 8 hours;
3. the solution is tested to contain no iodine, and is put into a 5L separating funnel to be kept stand for layering, and the treatment time is 5 hours;
5. discharging the lower layer liquid and collecting the upper layer liquid;
6. centrifuging the supernatant at 4000RPM for 60 min;
7. and after the centrifugation is finished, taking the supernatant after the centrifugation treatment, namely the high-purity pyrazine compound solution.
Comparative example 1
1. Taking 500g of pyrazine compound solution, 100g of silver carbonate powder and 2L of a three-mouth glass bottle;
2. mixing the two, stirring for 2h, standing and settling;
3. the solution was tested for iodine.
Comparative example 2
1. 500g of pyrazine compound solution, 100g of silver carbonate powder and 2L of three-mouth glass bottle;
2. mixing the two, stirring for 5h, standing and settling;
3. the solution was tested for iodine.
Comparative example 3:
1. 500g of pyrazine compound solution, 100g of silver carbonate powder and 2L of three-mouth glass bottle;
2. mixing the two, putting into 70 ℃ water bath, stirring for 2h, standing and settling;
3. the solution was tested to contain a small amount of iodine.
As shown in comparative examples 1 and 2, after adding the silver carbonate powder to the pyrazine compound solution, if the mixture is merely mixed and stirred, and left to stand for settling, the obtained pyrazine compound solution still contains iodine, and the purity thereof is not high; as shown in comparative example 3, when the time required for adding the silver carbonate powder to the pyrazine compound solution was short (2 hours), the mixture was merely heated in a water bath and stirred, and left to settle, a small amount of iodine was still contained in the obtained pyrazine compound solution.
As shown in example 1, after adding the silver carbonate powder into the pyrazine compound solution, the mixture is first heated in a water bath, mixed and stirred for a long time (8 hours), so that the pyrazine compound solution does not contain iodine, and meanwhile, after the pyrazine compound solution is still placed and settled, the pyrazine compound solution is centrifuged, so that the purity of the finally obtained pyrazine compound solution is high. In addition, the application further tests the high-purity pyrazine compound solution prepared in example 1, and the light modulation film prepared by using the high-purity pyrazine compound solution has the haze of 5-10% which is basically invisible to naked eyes, so that the haze requirement of the prior art on the light modulation film can be met.
To sum up, this application provides a method of getting rid of impurity iodine among pyrazine compound, through adding silver carbonate powder in the pyrazine compound solution that contains impurity iodine, make impurity iodine and silver carbonate powder produce chemical reaction and generate other substances to clear away the impurity iodine among the pyrazine compound solution, reach the purpose of getting rid of impurity iodine among the pyrazine compound fast, and utilize the haze of the light adjusting film of the pyrazine compound preparation that this application prepared to reduce to about 5%.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
While the present embodiments have been described with reference to the accompanying drawings, it is to be understood that the invention is not limited to the precise embodiments described above, which are meant to be illustrative and not restrictive, and that various changes may be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. A method for removing impurity iodine in pyrazine compounds is characterized by comprising the following steps:
(a) placing a pyrazine compound containing impurity iodine and isoamyl acetate into a three-neck flask, heating the three-neck flask, stirring the pyrazine compound and the isoamyl acetate to dissolve the pyrazine compound into the isoamyl acetate to form a pyrazine compound solution containing impurity iodine, wherein the mode of heating the three-neck flask is water bath heating, the water bath heating temperature is 70 ℃, the speed of stirring the pyrazine compound and the isoamyl acetate is 300 r/min, and the dissolving time of the pyrazine compound is 8 hours;
(b) adding silver carbonate powder into the pyrazine compound solution, heating the pyrazine compound solution, and enabling the silver carbonate powder to react with impurity iodine in the pyrazine compound solution to form a mixed solution;
(c) carrying out sedimentation treatment on the mixed solution;
(d) and centrifuging the settled supernatant after the settlement is finished to obtain a pyrazine compound solution without impurity iodine.
2. A method for removing iodine impurity from pyrazine compound according to claim 1, wherein the temperature of the pyrazine compound solution is 70 ℃ during the step (b).
3. The method for removing iodine impurity from pyrazine compound according to claim 1, wherein the step (b) of heating the pyrazine compound solution further comprises the step of performing an iodine-containing test on the pyrazine compound solution.
4. The method for removing impurity iodine from pyrazine compound according to claim 3, wherein the method for iodine test comprises the following steps:
preparing a starch solution;
and taking part of the pyrazine compound solution, adding the pyrazine compound solution into the starch solution, if the starch solution turns yellow, judging that iodine still exists in the pyrazine compound solution, continuing to heat the pyrazine compound solution, otherwise, judging that iodine does not exist in the pyrazine compound solution, and stopping heating the pyrazine compound solution.
5. The method for removing iodine impurity from pyrazine compound according to claim 1, wherein the step (c) further comprises discharging a lower solution and collecting the upper solution after the mixed solution is subjected to sedimentation treatment.
6. The method for removing iodine impurity from pyrazine compound according to claim 1, wherein in step (d), the centrifugation speed of the supernatant is 4000rpm and the centrifugation time is 60 minutes.
7. The method for removing impurity iodine from pyrazine compound according to claim 1, wherein in step (d), the supernatant after centrifugation is collected after the supernatant is centrifuged, and the supernatant is the pyrazine compound solution without impurity iodine.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109134389A (en) * | 2018-09-21 | 2019-01-04 | 江苏铁锚玻璃股份有限公司 | The purification process of 2,5- pyrazine dicarboxylic acids and obtained 2,5- pyrazine dicarboxylic acids |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109134389A (en) * | 2018-09-21 | 2019-01-04 | 江苏铁锚玻璃股份有限公司 | The purification process of 2,5- pyrazine dicarboxylic acids and obtained 2,5- pyrazine dicarboxylic acids |
Non-Patent Citations (2)
| Title |
|---|
| Development of silver nanoparticle–doped adsorbents for the separation and recovery of radioactive iodine from alkaline solutions;Taewoon Kim等;《Applied Radiation and Isotopes》;20170719;第129卷;215–221 * |
| 高效吸附碘材料的制备及其吸附性能和机理研究;余芳;《青海师范大学硕士学位论文》;20191231;1-64 * |
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