CN1389449A - Electron-level ammonium citrate and its production process - Google Patents
Electron-level ammonium citrate and its production process Download PDFInfo
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- CN1389449A CN1389449A CN 02137975 CN02137975A CN1389449A CN 1389449 A CN1389449 A CN 1389449A CN 02137975 CN02137975 CN 02137975 CN 02137975 A CN02137975 A CN 02137975A CN 1389449 A CN1389449 A CN 1389449A
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- ammonium citrate
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Abstract
The present invention discloses a kind of electronic-grade ammonium citrate and its production method. In its product the content of ammonium citrate is greater than or equal to 99%, and its production method includes the steps of first reaction, forerunning, second reaction, rectification, condensation and crystallization, separation and extraction and vacuum drying. As compared with reagent-grade ammonium citrate the inpurity index of said invented product is less by several tenfold. It can be used as cleaning agent in high-pressure foil-forming process, and its cleaning efficiency is high, at the same time the structure and performance of the treated anodic oxidation film are obviously improved, and when said invented product is used as medium in aluminium electrolytic capacitor, its performance is stable, and the service life of capacitor can be raised.
Description
Technical field:
The present invention relates to a kind of ammonium citrate.
Background technology:
Ammonium citrate changes into paper tinsel and produces supporting material as a kind of aluminium electrolutic capacitor and mesohigh of being applied to, and prior art generally adopts the lemon ammonium of SILVER REAGENT, and its impurity is many, and when being used for mesohigh and changing into paper tinsel as clean-out system, cleaning efficiency is not high.
Summary of the invention:
The object of the present invention is to provide a kind of impurity is few, content is high electronic-grade ammonium citrate and production method.
Technical solution of the present invention is:
A kind of electronic-grade ammonium citrate, its feature: the content of ammonium citrate 〉=99%.
Above-mentioned electronic-grade ammonium citrate, Cl
-＜0.0001%, SO
4 2-＜0.0020%, Fe
3+＜0.0005%, heavy metal＜0.0005%.
A kind of production method of electronic-grade ammonium citrate, its feature: comprise the following steps: successively
1. the citric acid raw material is carried out primary first-order equation with gas ammonia under the water existence condition, be reflected at and carry out on active-carbon bed, it is auxiliary agent that potassium permanganate is adopted in reaction;
2. the reaction solution that 1. step is obtained is flowed through and is had the yin, yang ion exchange resin bed of strongly acidic styrene's series Zeo-karb and strong-basicity styrene series row anionite-exchange resin, and carries out fore-running, condensation;
3. will carry out secondary reaction with gas ammonia through the solution after 2. handling, be auxiliary combination agent with zinc granule during reaction;
4. the solution that secondary reaction is obtained carries out rectifying, condensation-crystallization is handled, and extracts in skimmer again, promptly gets product through vacuum-drying then.
The 1. middle gas ammonia feeding amount of step is 20%～35% of a citric acid amount.Step 3. in, during secondary reaction, gas ammonia feeding amount is 20%～35% of a citric acid material quantity, the zinc granule amount is 2%～3% of a citric acid material quantity.The 1. middle citric acid raw material employing of step content is 98～99% citric acid, and the hydromining specific conductivity is the pure water of 16～18 megaohms.The temperature of primary first-order equation is 50～65 ℃, and the time is 20～60 minutes, and the secondary reaction temperature is 60～90 ℃, and the time is 60～100 minutes.
Product provided by the invention is littler tens of times than SILVER REAGENT ammonium citrate impurity index, being applied to mesohigh changes in the paper tinsel as clean-out system, has the cleaning efficiency height, than advantages such as clean-out system consumptions such as electronic-grade citric acid lack, thereby reduced the cleaning cost, the structure of the anode oxide film after handling simultaneously and performance be improved significantly, the anode foils specific volume improves 25～50%, and makes energy consumption reduction by 30～50% in the anode foils process.When product of the present invention uses as medium in aluminium electrolutic capacitor, stable performance, electric capacity is improved work-ing life.
The invention will be further described below in conjunction with embodiment.
Embodiment:
Embodiment:
1. the citric acid raw material is carried out primary first-order equation with gas ammonia under the water existence condition, be reflected at and carry out on active-carbon bed, it is auxiliary agent that potassium permanganate is adopted in reaction, gas ammonia feeding amount is 20%～a 35% (example 20% of citric acid amount, 25%, 30%, 35%), it is 98～99% (examples 98% that the citric acid raw material adopts content, 98.5%, 99%) citric acid, the hydromining specific conductivity is 16～18 megaohms (examples 16,17,18) pure water, the temperature of primary first-order equation is 50～65 ℃ of (examples 50,55,60,65 ℃), the time is 20～60 minutes (examples 20,30,40,50,60 minutes).
2. the reaction solution that 1. step is obtained uses under the pure water situation 1. identical with step, flow through and have the yin, yang ion exchange resin bed of strongly acidic styrene's series Zeo-karb and strong-basicity styrene series row anionite-exchange resin, carry out fore-running with the distillation tower then, remove impurity, make through the solution saturation ratio after the primary first-order equation to reach 50%～60%, re-use crystallizer and be condensed to room temperature;
3. will be through the solution after 2. handling, carry out secondary reaction with gas ammonia, be auxiliary combination agent with zinc granule during reaction, gas ammonia feeding amount is 1. 20%～35% (example 20%, 25%, 30%, 35%) of middle citric acid material quantity of step, the zinc granule amount is 2%～3% (example 2%, 2.5%, 3%) of citric acid material quantity, the secondary reaction temperature is 60～90 ℃ (60,70,80,90 ℃ of examples), and the time is 60～100 minutes (example 60,70,80,90,100 minutes).
4. the solution that secondary reaction is obtained carries out the rectifying impurity elimination, condensation-crystallization is handled in crystallizer, the condensation-crystallization treatment temp is 5～10 ℃ (5,8,10 ℃ of examples), 24～36 hours time (example 24,30,36 hours), in skimmer, extract again, temperature is 2～5 ℃ (2,3,4,5 ℃ of examples), then through vacuum-drying, during vacuum-drying, temperature is 90～105 ℃ (90,95,100,105 ℃ of examples), and vacuum tightness is 0.01MPa～0.02MPa, also through further being ground into 40～20 purpose particles, promptly get product, the packing warehouse-in.
The products obtained therefrom technical indicator is: the content of ammonium citrate 〉=99%, Cl
-＜0.0001%, SO
4 2-＜0.0020%, Fe
3+＜0.0005%, heavy metal＜0.0005%.
Claims (7)
1, a kind of electronic-grade ammonium citrate is characterized in that: the content of ammonium citrate 〉=99%.
2, electronic-grade ammonium citrate according to claim 1 is characterized in that: Cl
-＜0.0001%, SO
4 2-＜0.0020%, Fe
3+＜0.0005%, heavy metal＜0.0005%.
3, a kind of production method of electronic-grade ammonium citrate is characterized in that: comprise the following steps: successively
1. the citric acid raw material is carried out primary first-order equation with gas ammonia under the water existence condition, be reflected at and carry out on active-carbon bed, it is auxiliary agent that potassium permanganate is adopted in reaction;
2. the reaction solution that 1. step is obtained is flowed through and is had the yin, yang ion exchange resin bed of strongly acidic styrene's series Zeo-karb and strong-basicity styrene series row anionite-exchange resin, and carries out fore-running, condensation;
3. will carry out secondary reaction with gas ammonia through the solution after 2. handling, be auxiliary combination agent with zinc granule during reaction;
4. the solution that secondary reaction is obtained carries out rectifying, condensation-crystallization is handled, and extracts in skimmer again, promptly gets product through vacuum-drying then.
4, the production method of electronic-grade ammonium citrate according to claim 3 is characterized in that: the 1. middle gas ammonia feeding amount of step is 20%～35% of a citric acid amount.
5, the production method of electronic-grade ammonium citrate according to claim 3 is characterized in that: step 3. in, during secondary reaction, gas ammonia feeding amount is 20%～35% of a citric acid material quantity, the zinc granule amount is 2%～3% of a citric acid material quantity.
6, according to the production method of claim 3 or 4 described electronic-grade ammonium citrates, it is characterized in that: the 1. middle citric acid raw material employing of step content is 98～99% citric acid, and the hydromining specific conductivity is the pure water of 16～18 megaohms.
7, according to the production method of claim 3 or 4 described electronic-grade ammonium citrates, it is characterized in that: the temperature of primary first-order equation is 50～65 ℃, and the time is 20～60 minutes, and the secondary reaction temperature is 60～90 ℃, and the time is 60～100 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02137975 CN1246283C (en) | 2002-07-16 | 2002-07-16 | Electron-level ammonium citrate and its production process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02137975 CN1246283C (en) | 2002-07-16 | 2002-07-16 | Electron-level ammonium citrate and its production process |
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| CN1389449A true CN1389449A (en) | 2003-01-08 |
| CN1246283C CN1246283C (en) | 2006-03-22 |
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|---|---|---|---|
| CN 02137975 Expired - Fee Related CN1246283C (en) | 2002-07-16 | 2002-07-16 | Electron-level ammonium citrate and its production process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104447287A (en) * | 2014-12-22 | 2015-03-25 | 南通市飞宇精细化学品有限公司 | Preparation method of diammonium hydrogen citrate |
| CN106674232A (en) * | 2017-01-04 | 2017-05-17 | 湖南省正源储能材料与器件研究所 | Method for preparing high-purity spiral ammonium salt with ion exchange purification method |
| CN112593234A (en) * | 2020-12-03 | 2021-04-02 | 南通恒兴电子材料有限公司 | Preparation method of ammonium citrate |
-
2002
- 2002-07-16 CN CN 02137975 patent/CN1246283C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104447287A (en) * | 2014-12-22 | 2015-03-25 | 南通市飞宇精细化学品有限公司 | Preparation method of diammonium hydrogen citrate |
| CN106674232A (en) * | 2017-01-04 | 2017-05-17 | 湖南省正源储能材料与器件研究所 | Method for preparing high-purity spiral ammonium salt with ion exchange purification method |
| CN112593234A (en) * | 2020-12-03 | 2021-04-02 | 南通恒兴电子材料有限公司 | Preparation method of ammonium citrate |
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| Publication number | Publication date |
|---|---|
| CN1246283C (en) | 2006-03-22 |
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