CN102590443A - Safe stable type Karl Fischer reagent and preparation method thereof - Google Patents
Safe stable type Karl Fischer reagent and preparation method thereof Download PDFInfo
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- CN102590443A CN102590443A CN2012100576341A CN201210057634A CN102590443A CN 102590443 A CN102590443 A CN 102590443A CN 2012100576341 A CN2012100576341 A CN 2012100576341A CN 201210057634 A CN201210057634 A CN 201210057634A CN 102590443 A CN102590443 A CN 102590443A
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Abstract
The invention discloses a safe stable type Karl Fischer reagent which comprises the following components in percentage by mass: 60-64 percent of diethylene glycol monomethyl ether, 8-12 percent of diethanol amine, 3.5-5.5 percent of pyridine, 12-15 percent of sulfur dioxide and 8-12 percent of iodine. The preparation method of the safe stable type Karl Fischer reagent comprises the following steps of: adding the diethylene glycol monomethyl ether, the diethanol amine and the pyridine in a reaction kettle and mixing; introducing the sulfur dioxide; after the gas is introduced, cooling the mixed solution below 25DEG C; and adding the iodine and stirring the mixed solution until the iodine is completely dissolved and obtaining a target product. According to the safe stable type Karl Fischer reagent and the preparation method thereof disclosed by the invention, original poisonous dangerous solvent is replaced by a safety type solvent, so that the safe stable type Karl Fischer reagent is non-poisonous, safe, environment-friendly and stable in quality; and after the safe stable type Karl Fischer reagent is stored for a long time, the titer is still within a usable range.
Description
Technical field
The present invention relates to chemical field, particularly relate to a kind of safety and stability type karl Fischer reagent and preparation method thereof.
Background technology
Karl Fischer reagent (Karl-Fischer Reagent); Claim Ka Shi reagent again; Be a kind of common agents of assay determination liquid water content, have very at neighborhoods such as medicine, chemical industry, petroleum refining and use widely that measuring moisture with the karl Fischer method is international, domestic generally acknowledged universal method.
Existing karl Fischer reagent is the mix reagent of pyridine, methyl alcohol, iodine and sulphuric dioxide, wherein owing to the pyridine foul smelling, and operating environment of pollution; The toxicity of methyl alcohol is big, is detrimental to health, and poor storage stability, standing time is short, and inflammable.Thereby existing this type karl Fischer reagent is the one-level flammable liquid, and buying, transportation, storage are all had strict demand, and harmful to user of service's health, is unfavorable for environmental protection.
Summary of the invention
The technical matters that the present invention mainly solves provides a kind of safety and stability type karl Fischer reagent and preparation method thereof, safety and environmental protection, steady quality.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of safety and stability type karl Fischer reagent is provided, it is characterized in that, its mass percent is formed and is comprised:
Diethylene glycol dimethyl ether 60～64%
Diethanolamine 8～12%
Pyridine 3.5～5.5%
Sulphuric dioxide 12～15%
Iodine 8～12%.
For solving the problems of the technologies described above; Another technical scheme that the present invention adopts is: the preparation method of safety and stability type karl Fischer reagent is provided, and detailed process is following: in agitated reactor, add the diethylene glycol dimethyl ether mass percent and be 60～64%, the diethanolamine mass percent is 8～12%, the pyridine mass percent is 3.5～5.5% to mix; In mixed solution, feeding the sulphuric dioxide mass percent is 12～15%; Ventilation finishes, and is chilled to below 25 ℃, and adding iodine quality number percent is 8～12%; Be stirred to whole dissolvings, promptly obtain target product.
In preferred embodiment of the present invention, after said sulphuric dioxide ventilation finished, control semi-manufacture pH value was 4～7.
In preferred embodiment of the present invention, be cooled to 10～15 ℃, slowly add iodine, and make that temperature is no more than 15 ℃ in the course of reaction.
The invention has the beneficial effects as follows: safety and stability type karl Fischer reagent of the present invention and preparation method thereof; Adopt the safety-type solvent to replace original poisonous dangerous flux, nontoxic, safety, environmental protection, and steady quality; After long-time the storage, titer is still in spendable scope.
Description of drawings
Fig. 1 is the process chart of safety and stability type karl Fischer reagent preparation method of the present invention one preferred embodiment.
Embodiment
Below in conjunction with accompanying drawing preferred embodiment of the present invention is set forth in detail, thereby protection scope of the present invention is made more explicit defining so that advantage of the present invention and characteristic can be easier to it will be appreciated by those skilled in the art that.
In conjunction with shown in Figure 1, safety and stability type karl Fischer reagent preparation method one preferred embodiment technological process of the present invention is following:
1, hybrid reaction
In the 100L agitated reactor, add diethylene glycol dimethyl ether 65kg, under agitation add diethanolamine 10kg and pyridine 5kg, stirring and evenly mixing 10 minutes.
2, in the solution of mixing, slowly feed sulphuric dioxide 14kg, cool off simultaneously.Ventilation finishes, middle control check PH to 4～7.
3, the semi-manufacture that are up to the standards of middle control are cooled to 10～15 ℃, slowly add iodine 10kg, make that temperature is no more than 15 ℃ in the course of reaction.
4, add iodine and finish after, keep 10～15 ℃ of temperature, and stir and promptly get karl Fischer reagent.
5, semi-manufacture censorships qualified after, packing, product inspection warehousing after passing.
The quality index of karl Fischer reagent of the present invention
| Project | Index |
| Titer, mg/ml | 3～5 |
| PH(25℃) | 4～7 |
| Stability, min >;= | 5 |
The detection method of karl Fischer reagent:
1, titer
In reaction bulb, add the methyl alcohol (submergence platinum electrode) of certain volume, under agitation use the karl Fischer reagent titration to terminal, this moment, the consumption of karl Fischer was disregarded.With the accurate microsyringe of 10ul, accurately draw 10ul (10mg) water, continue to terminal with the karl Fischer reagent titration.(reservation solution)
The titer T of karl Fischer reagent, numerical value represent that with mg/ml the result is calculated as follows:
m
T?= ————
V
In the formula: m---the numerical value of the quality of water, mg;
The numerical value of the volume of V---karl Fischer reagent, ml.
2、PH
Pressing the regulation of GB/T 9724-2007 measures.Wherein measure the 100ml sample, using precision acidity meter to measure PH is 4～7.
3, stability
With the solution of the 1st reservation, observe the terminal point numerical value (or color of terminal point solution) on the moisture teller, should remain in the 5min constant.
Safety and stability type karl Fischer reagent preparation method of the present invention has safety, stable, environmental protection, advantage that processing cost is lower, is suitable for the batch process of chemical reagent chemical enterprise.The present invention is on original karl Fischer reagent production technology basis; Raw material has been carried out the adjustment of reasonable science, selected non-hazardous chemical as raw material, and the adjustment proportioning raw materials; Not only save production cost but also can improve product yield, reached the effect of safety and environmental protection.Titration reagent as measuring micro-moisture has the terminal point good stability, the result precision advantages of higher.Improve breadboard working environment, guarantee that the analyst's is healthy.
The above is merely embodiments of the invention; Be not so limit claim of the present invention; Every equivalent structure or equivalent flow process conversion that utilizes instructions of the present invention and accompanying drawing content to be done; 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 (4)
1. a safety and stability type karl Fischer reagent is characterized in that, its mass percent is formed and comprised:
Diethylene glycol dimethyl ether 60～64%
Diethanolamine 8～12%
Pyridine 3.5～5.5%
Sulphuric dioxide 12～15%
Iodine 8～12%.
2. the preparation method of a safety and stability type karl Fischer reagent is characterized in that detailed process is following: in agitated reactor; Add the diethylene glycol dimethyl ether mass percent and be 60～64%, the diethanolamine mass percent is 8～12%, the pyridine mass percent is 3.5～5.5% to mix, in mixed solution, feeding the sulphuric dioxide mass percent is 12～15%, ventilation finishes; Be chilled to below 25 ℃; Adding iodine quality number percent is 8～12%, is stirred to whole dissolvings, promptly obtains target product.
3. the preparation method of safety and stability type karl Fischer reagent according to claim 2 is characterized in that, after said sulphuric dioxide ventilation finished, control semi-manufacture pH value was 4～7.
4. the preparation method of safety and stability type karl Fischer reagent according to claim 2 is characterized in that, is cooled to 10～15 ℃, slowly adds iodine, and makes that temperature is no more than 15 ℃ in the course of reaction.
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| CN2012100576341A CN102590443A (en) | 2012-03-07 | 2012-03-07 | Safe stable type Karl Fischer reagent and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102749401A (en) * | 2012-07-30 | 2012-10-24 | 山东阿如拉药物研究开发有限公司 | Quality inspection method of traditional Chinese medicine composition twenty-five-ingredient lung disease preparation |
| CN103308654A (en) * | 2013-06-13 | 2013-09-18 | 深圳市华星光电技术有限公司 | Solution and testing method for testing moisture content in photoresistance peeling liquid |
| CN106442862A (en) * | 2016-09-19 | 2017-02-22 | 东莞市杉杉电池材料有限公司 | Karl-Fischer reagent for electrolyte moisture detection and preparation method thereof |
| CN109254110A (en) * | 2018-09-30 | 2019-01-22 | 东莞市杉杉电池材料有限公司 | A kind of lithium-ion battery electrolytes water content detection karl Fischer reagent and preparation method thereof |
| CN109374822A (en) * | 2018-11-08 | 2019-02-22 | 赛孚瑞化工邯郸有限公司 | Lithium electricity industry water content detection karl Fischer reagent and preparation method thereof |
| CN109406713A (en) * | 2018-11-22 | 2019-03-01 | 东莞市杉杉电池材料有限公司 | A kind of karl Fischer volumetric method reagent and its preparation method and application |
| CN110095563A (en) * | 2018-01-27 | 2019-08-06 | 深圳新宙邦科技股份有限公司 | A kind of karl Fischer reagent |
| CN112567240A (en) * | 2018-07-25 | 2021-03-26 | 霍尼韦尔国际公司 | Method for determining moisture content in sample using imidazole derivative and hydrogen halide donor |
| CN112684101A (en) * | 2020-12-01 | 2021-04-20 | 赛孚瑞化工邯郸有限公司 | Coulomb method Karl Fischer reagent special for Karl furnace and preparation method thereof |
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|---|---|---|---|---|
| US4354853A (en) * | 1981-05-11 | 1982-10-19 | Harald Dahms | Karl Fischer reagent and its use |
| EP1207389A1 (en) * | 2000-11-15 | 2002-05-22 | Sigma-Aldrich Laborchemikalien GmbH | Karl-Fischer-Reagent |
| CN1793907A (en) * | 2005-11-15 | 2006-06-28 | 上海新中化学科技有限公司 | Safety karl Fischer reagent and its preparation method |
| CN101256178A (en) * | 2008-04-17 | 2008-09-03 | 上海化学试剂研究所 | Non-pyridine karl fischer agent as well as preparing method |
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2012
- 2012-03-07 CN CN2012100576341A patent/CN102590443A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4354853A (en) * | 1981-05-11 | 1982-10-19 | Harald Dahms | Karl Fischer reagent and its use |
| EP1207389A1 (en) * | 2000-11-15 | 2002-05-22 | Sigma-Aldrich Laborchemikalien GmbH | Karl-Fischer-Reagent |
| CN1793907A (en) * | 2005-11-15 | 2006-06-28 | 上海新中化学科技有限公司 | Safety karl Fischer reagent and its preparation method |
| CN101256178A (en) * | 2008-04-17 | 2008-09-03 | 上海化学试剂研究所 | Non-pyridine karl fischer agent as well as preparing method |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102749401A (en) * | 2012-07-30 | 2012-10-24 | 山东阿如拉药物研究开发有限公司 | Quality inspection method of traditional Chinese medicine composition twenty-five-ingredient lung disease preparation |
| CN103308654A (en) * | 2013-06-13 | 2013-09-18 | 深圳市华星光电技术有限公司 | Solution and testing method for testing moisture content in photoresistance peeling liquid |
| CN103308654B (en) * | 2013-06-13 | 2016-08-10 | 深圳市华星光电技术有限公司 | For testing the method for moisture in photoresistance stripper |
| CN106442862A (en) * | 2016-09-19 | 2017-02-22 | 东莞市杉杉电池材料有限公司 | Karl-Fischer reagent for electrolyte moisture detection and preparation method thereof |
| CN110095563A (en) * | 2018-01-27 | 2019-08-06 | 深圳新宙邦科技股份有限公司 | A kind of karl Fischer reagent |
| CN112567240A (en) * | 2018-07-25 | 2021-03-26 | 霍尼韦尔国际公司 | Method for determining moisture content in sample using imidazole derivative and hydrogen halide donor |
| CN109254110A (en) * | 2018-09-30 | 2019-01-22 | 东莞市杉杉电池材料有限公司 | A kind of lithium-ion battery electrolytes water content detection karl Fischer reagent and preparation method thereof |
| CN109374822A (en) * | 2018-11-08 | 2019-02-22 | 赛孚瑞化工邯郸有限公司 | Lithium electricity industry water content detection karl Fischer reagent and preparation method thereof |
| CN109406713A (en) * | 2018-11-22 | 2019-03-01 | 东莞市杉杉电池材料有限公司 | A kind of karl Fischer volumetric method reagent and its preparation method and application |
| CN112684101A (en) * | 2020-12-01 | 2021-04-20 | 赛孚瑞化工邯郸有限公司 | Coulomb method Karl Fischer reagent special for Karl furnace and preparation method thereof |
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Application publication date: 20120718 |