CN107741448A - The detection method of content of degradation impurity in magnesium alkoxide compound - Google Patents
The detection method of content of degradation impurity in magnesium alkoxide compound Download PDFInfo
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- CN107741448A CN107741448A CN201711091212.5A CN201711091212A CN107741448A CN 107741448 A CN107741448 A CN 107741448A CN 201711091212 A CN201711091212 A CN 201711091212A CN 107741448 A CN107741448 A CN 107741448A
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- magnesium
- alkoxide compound
- magnesium alkoxide
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- 239000011777 magnesium Substances 0.000 title claims abstract description 48
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 47
- -1 magnesium alkoxide compound Chemical class 0.000 title claims abstract description 46
- 239000012535 impurity Substances 0.000 title claims abstract description 34
- 230000015556 catabolic process Effects 0.000 title claims abstract description 18
- 238000006731 degradation reaction Methods 0.000 title claims abstract description 18
- 238000001514 detection method Methods 0.000 title abstract description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 25
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000004448 titration Methods 0.000 claims abstract description 20
- 229960000583 acetic acid Drugs 0.000 claims abstract description 11
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 8
- RVDLHGSZWAELAU-UHFFFAOYSA-N 5-tert-butylthiophene-2-carbonyl chloride Chemical compound CC(C)(C)C1=CC=C(C(Cl)=O)S1 RVDLHGSZWAELAU-UHFFFAOYSA-N 0.000 claims description 19
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 19
- 239000000347 magnesium hydroxide Substances 0.000 claims description 19
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 5
- CRGZYKWWYNQGEC-UHFFFAOYSA-N magnesium;methanolate Chemical compound [Mg+2].[O-]C.[O-]C CRGZYKWWYNQGEC-UHFFFAOYSA-N 0.000 claims description 4
- WNJYXPXGUGOGBO-UHFFFAOYSA-N magnesium;propan-1-olate Chemical compound CCCO[Mg]OCCC WNJYXPXGUGOGBO-UHFFFAOYSA-N 0.000 claims description 4
- ORPJQHHQRCLVIC-UHFFFAOYSA-N magnesium;propan-2-olate Chemical compound CC(C)O[Mg]OC(C)C ORPJQHHQRCLVIC-UHFFFAOYSA-N 0.000 claims description 4
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 abstract description 4
- 238000012827 research and development Methods 0.000 abstract description 2
- 239000003381 stabilizer Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 239000011654 magnesium acetate Substances 0.000 description 1
- XDKQUSKHRIUJEO-UHFFFAOYSA-N magnesium;ethanolate Chemical compound [Mg+2].CC[O-].CC[O-] XDKQUSKHRIUJEO-UHFFFAOYSA-N 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/42—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte
- G01N27/44—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte using electrolysis to generate a reagent, e.g. for titration
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention discloses a kind of detection method of degradation impurity in magnesium alkoxide compound, including：Step 1, enough methanol not mistake electrode is added in the titration cup of Cattell volumetric method titrator, be titrated to current potential terminal with karl Fischer titrant (KF), be totally consumed moisture therein；Step 2, continue to add excessive glacial acetic acid into titration cup, after instrument stabilizer, precision weighs appropriate magnesium alkoxide compound sample and is added in titration cup, reacts；After step 3, question response, current potential terminal is titrated to karl Fischer titrant (KF), is totally consumed moisture therein.Compared with titrating the detection method of magnesium elements in the prior art, detection method provided by the invention can more accurately detect the content of degradation impurity in magnesium alkoxide compound.Compared to such as taking using testing, the whether qualified detection method of raw material is judged by the means of lab scale, can save plenty of time and reagent cost using the method for the present invention, improve overall efficiency of research and development.
Description
Technical Field
The invention relates to the field of impurity analysis and detection of chemical reagents, in particular to a method for detecting degradation impurities in magnesium alkoxide.
Background
Magnesium alkoxide Mg (OR)2Wherein R is alkyl, and is a metal alkoxide compound, and the representative compounds comprise magnesium methoxide, magnesium ethoxide, magnesium isopropoxide, magnesium n-propoxide and the like. The magnesium alkoxide compounds are widely applied to inorganic synthesis, organic synthesis, directional catalytic polymerization, preparation of functional materials and the like, and are important chemical raw materials and reagents. At present, domestic literature reports on magnesium alkoxide compounds mainly focus on synthesis, preparation, purification and the like, and few literature reports on content determination of related impurities in magnesium alkoxide compounds are available. However, magnesium alkoxide compounds are easily contacted with water in the air during storage, transportation, and the like, and are slowly degraded, thereby generating degradation impurities mainly comprising magnesium hydroxide. These degradation impurities not only reduce the content of the magnesium alkoxide compound, but also more importantly affect the reactivity of the reagent, resulting in poor reaction yield or even no reaction.
At present, the quality of the reagent for detecting the magnesium alkoxide compound is determined by titrating the content of magnesium element. But the degradation impurities such as magnesium hydroxide and the like generated by the degradation of the magnesium alkoxide are also counted in the total magnesium content, so that the content detection result is inaccurate. On the other hand, if the magnesium alkoxide compound is tested to be qualified by means of a test or the like, the method has the defects of high cost, low efficiency and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for detecting the content of degradation impurities in a magnesium alkoxide compound, which can overcome the defects of inaccurate detection result, high cost, low efficiency and the like in the prior art.
In order to solve the technical problem, the method for detecting the degradation impurities in the magnesium alkoxide compound comprises the following steps:
step 1, adding sufficient methanol into a titration cup of a titration apparatus of a Karl-volumetric method, and titrating the methanol to a potential end point by using a Karl-Fischer titrant (KF) so as to completely consume water in the titration cup; if no special requirement exists, the drift value should be less than or equal to 30.
Step 2, continuously adding excessive glacial acetic acid into the titration cup, precisely weighing a proper amount of magnesium alkoxide compound sample after the instrument is stabilized, adding the magnesium alkoxide compound sample into the titration cup, and reacting; at this time, the magnesium hydroxide in the sample of the magnesium alkoxide compound reacts with the excess acetic acid previously added in a ratio of 1 to 2 to produce water, but the magnesium alkoxide compound itself does not react with the acetic acid.
The reaction formula is as follows:
Mg(OH)2+2CH3COOH＝Mg(CH3COO)2+2H2O。
and 3, after the reaction is finished, titrating to a potential end point by using a Karl-Fischer titrant (KF) to completely consume the water in the solution. And (3) calculating the molar weight of the water produced in the step (2) according to the consumption of a Karl-Fischer titrant (KF) in the step (3), calculating the molar weight of magnesium hydroxide according to a reaction equation in the step (2), multiplying the molar weight of the magnesium hydroxide by the molecular weight of the magnesium hydroxide, and dividing the molecular weight by the weighing amount of the magnesium alkoxide compound to obtain the content of magnesium hydroxide impurities in the magnesium alkoxide compound sample.
Specifically, the magnesium alkoxide compound is at least one selected from magnesium methoxide, magnesium ethoxide, magnesium isopropoxide and magnesium n-propoxide.
Specifically, when the magnesium alkoxide compound is magnesium ethoxide, the content of degradation impurities in a sample of the magnesium alkoxide compound is calculated according to the following formula: wImpurities＝1.62×WMoisture content(ii) a Wherein,
WimpuritiesRepresents the mass percentage (%) of degradation impurities (in terms of magnesium hydroxide) in the magnesium alkoxide compound;
1.62 denotes: in this reaction, 2 moles of water were reacted for every 1 mole of magnesium hydroxide, and the molecular weight of 1 mole of magnesium hydroxide was divided by the molecular weight of 2 moles of water to give 1.62;
Wmoisture contentRepresents the moisture content (%) of the magnesium alkoxide compound read by the instrument software after adding the magnesium ethoxide to the titration cup.
Specifically, the steps 1 to 3 are carried out in parallel to determine two copies.
Specifically, the excess glacial acetic acid in the step 2 is relative to a proper amount of a magnesium alkoxide compound sample; for example, glacial acetic acid is 4mL, and magnesium ethoxide is 0.2 g.
Magnesium ethoxide is generally used as a key raw material required by synthesis in medicine and chemical industry. After the raw materials are purchased, the process has equivalent requirements on the feeding amount, and then the detection of the content of impurities in the raw materials is crucial. And no relevant method or scheme is found through the early search.
Compared with the method for titrating magnesium element in the prior art, the detection method provided by the invention can more accurately detect the content of degradation impurities in the magnesium alkoxide compound. If the use test is adopted and the raw materials are judged to be qualified by means of a small test, a considerable time is needed for waiting for the reaction to be finished while consuming a large amount of samples. The method of the invention can save a large amount of time and the cost of purchasing samples, and improve the overall research and development efficiency. The method can also be applied to the detection of the degradation of impurities generated by contacting with water in the raw materials such as magnesium methoxide, magnesium propoxide, magnesium isopropoxide and the like.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Adding sufficient methanol or other suitable solvent into a titration cup of a Karl volumetric titrator to ensure that the titration cup is submerged, and titrating by using KF titrant to a potential end point to ensure that the water in the titration cup is completely consumed. If no special requirement exists, the drift value should be less than or equal to 30.
Adding 4mL of glacial acetic acid into a titration cup, precisely weighing about 0.2g of magnesium ethoxide sample after the instrument is stabilized (the sample amount can be properly adjusted), inputting 'weight (mg)' and corresponding sample information, and titrating to an end point.
Unless otherwise specified, two replicates were assayed.
The impurity content in the magnesium ethoxide sample is calculated according to the following formula:
Wimpurities＝1.62×WMoisture content
WImpurities: the mass percent of impurities (calculated as magnesium hydroxide) in the magnesium ethoxide is%
WMoisture contentRepresents the moisture content (in mass percent,%) of the magnesium alkoxide compound read by the instrument software after the magnesium ethoxide is added into the titration cup
The specific embodiment is as follows:
detecting the mass of a certain batch of magnesium ethoxide: the samples were taken 2 times, the mass of magnesium ethoxide added to the titration cup was 0.20294g and 0.20161g, respectively, and the moisture content read from the Karl-Fischer instrument software was 1.45% and 1.56%, respectively. Substituting the water content distribution for 2 times into the formula to obtain magnesium ethylate with impurity content respectively as follows: 2.35% and 2.53%. The average value of the impurity contents of the two parts is taken to obtain that the impurity content (calculated by magnesium hydroxide) of the magnesium ethoxide in the batch is 2.44 percent.
And the content of magnesium ethoxide, namely COA of the supplier, is more than 98.5 percent, and the content of the measured impurities is 2.44 percent, so that the batch of magnesium ethoxide is judged to be unqualified.
In summary, the above embodiments are merely preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A method for detecting degradation impurities in a magnesium alkoxide compound is characterized by comprising the following steps:
step 1, adding sufficient methanol into a titration cup of a titration apparatus of a Karl-volumetric method and enabling the methanol to submerge an electrode, and titrating the methanol to a potential end point by using a Karl-Fischer titrant to ensure that the water in the methanol is completely consumed;
step 2, continuously adding excessive glacial acetic acid into the titration cup, precisely weighing a proper amount of magnesium alkoxide compound sample after the instrument is stabilized, adding the magnesium alkoxide compound sample into the titration cup, and reacting;
and 3, after the reaction is finished, titrating to a potential end point by using a Karl-Fischer titrant to completely consume the water in the solution.
2. The method of claim 1, wherein the magnesium alkoxide compound is selected from at least one of magnesium methoxide, magnesium ethoxide, magnesium isopropoxide, and magnesium n-propoxide.
3. The method of claim 2, wherein when the magnesium alkoxide compound is magnesium ethoxide, the level of degradation impurities in the magnesium alkoxide compound sample is calculated according to the following formula: wImpurities＝1.62×WMoisture content(ii) a Wherein, WImpuritiesRepresents the mass percentage (%) of degradation impurities (in terms of magnesium hydroxide) in the magnesium alkoxide compound; wMoisture contentRepresents the water content (%) of the magnesium alkoxide compound read by the instrument after adding the magnesium ethoxide to the titration cup.
4. The method of claim 1, wherein steps 1-3 are performed in parallel.
5. The method of claim 1, wherein the excess glacial acetic acid in step 2 is relative to an appropriate amount of sample magnesium alkoxide.
6. The method of claim 5, wherein the glacial acetic acid is 4mL and the magnesium ethoxide is 0.2 g.
7. The method of claim 1, wherein in step 2, the magnesium hydroxide in the sample of the magnesium alkoxide compound reacts with the excess acetic acid previously added in a ratio of 1 to 2 to produce water.
8. The method according to claim 1, wherein in the step 3, the molar weight of the water produced in the step 2 is calculated according to the consumption of the Karl-Fischer titrant in the step 3, the molar weight of the magnesium hydroxide is calculated according to the reaction equation in the step 2, and the content of the magnesium hydroxide impurity in the magnesium alkoxide compound sample is obtained by dividing the molar number of the magnesium hydroxide by the molecular weight of the magnesium hydroxide by the weighing amount of the magnesium alkoxide compound.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109298127A (en) * | 2018-10-19 | 2019-02-01 | 常州合全药业有限公司 | The detection method of impurity content is condensed in alkylsilanol |
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| US20050131257A1 (en) * | 2003-12-13 | 2005-06-16 | Burkhard Standke | Process for preparing alkoxy-pure alkaline earth alkoxides |
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Patent Citations (1)
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| US20050131257A1 (en) * | 2003-12-13 | 2005-06-16 | Burkhard Standke | Process for preparing alkoxy-pure alkaline earth alkoxides |
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| 周德星 等: "卡尔·费休法测定乙氧基镁中氢氧化镁的含量", 《沈阳化工》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109298127A (en) * | 2018-10-19 | 2019-02-01 | 常州合全药业有限公司 | The detection method of impurity content is condensed in alkylsilanol |
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