CN109211718A - K in potassium bichromate production2The measuring method of O content - Google Patents

K in potassium bichromate production2The measuring method of O content Download PDF

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Publication number
CN109211718A
CN109211718A CN201811258910.4A CN201811258910A CN109211718A CN 109211718 A CN109211718 A CN 109211718A CN 201811258910 A CN201811258910 A CN 201811258910A CN 109211718 A CN109211718 A CN 109211718A
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potassium
solution
content
tetraphenylborate
gained
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CN201811258910.4A
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CN109211718B (en
Inventor
卢国美
廖荣
黄国强
马丹
段静
李超雄
苏晓亮
曹嵩
商琴
王松
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HUBEI ZHENHUA CHEMICAL CO Ltd
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HUBEI ZHENHUA CHEMICAL CO Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34—Purifying; Cleaning
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38—Diluting, dispersing or mixing samples
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/42—Low-temperature sample treatment, e.g. cryofixation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44—Sample treatment involving radiation, e.g. heat
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/02—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using precipitation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38—Diluting, dispersing or mixing samples
    • G01N2001/386—Other diluting or mixing processes

Abstract

The invention discloses K in a kind of production of potassium bichromate2The measuring method of O content takes potassium bichromate reaction solution V to be measured, and in acid condition plus Cr VI is all reduced to trivalent chromium by reducing agent, adds alkali neutralization to solution to be in neutrality, 1-2h, filtration washing to no K are kept the temperature at a temperature of 90-100 DEG C+Until, collect cleaning solution；Potassium tetraphenylborate precipitating generates: gained cleaning solution is heated to boiling, sodium tetraphenylborate solution is added dropwise under stirring condition and is precipitated to potassium tetraphenylborate is generated, cooling and standings；Step 2 gained coolant liquid is transferred to the G to dry to constant weight in 120 DEG C4It is filtered in glass sand core funnel, gained precipitating is washed dropping liquid with potassium tetraphenylborate and washed, and the W that dries to constant weight finally is placed in drying box；K2A=0.1314 × W × 1000/V is calculated as follows in O content.

Description

K in potassium bichromate production2The measuring method of O content
Technical field
The invention belongs to technical field of chemical engineering, and in particular to K in a kind of production of potassium bichromate2The measurement side of O content Method.
Background technique
In potassium bichromate industrialized production, in order to ensure KCl100% is utilized, the additional amount of KCI is theoretical amount 98%, and Na2Cr2O7It is slightly excessive.After matching production a period of time by this, it will appear " thanks to " K in system+Phenomenon, or due to metering Etc. reasons also lead to K+/Cr6+Ratio disequilibrium, to influence to produce.It therefore, be periodically to the K in production system2Cr2O7、 K2The content of O is measured, to Instructing manufacture.
K in system2Cr2O7The measurement of content is to carry out redox measurement using iron ammonium sulfate, is a kind of comparison Classical method, which is not described herein again.
And K2The measuring principle of O content is K+It is reacted with sodium tetraphenylborate solution and generates potassium tetraphenylborate, washed, drying, weighing Afterwards, by the way that K is calculated2The content of O.Traditional method is after being restored Cr VI, neutralizing removing Cr VI, to add 10% Acetic acid adjust it is weakly acidic to solution, then plus the tetraphenylboron sodium ethanol solution of 0.1mol/L precipitated, be saturated with potassium tetraphenylborate After solution transfer, washing precipitating, dries to constant weight in 120 DEG C, K is figured out according to the formula2The content of O.
But during practice examining, the condition of potassium tetraphenylborate precipitating is difficult to control, when parallel determination, the tetraphenylboron of generation The amount of potassium precipitating is different, and errors of analytical results is very big.In order to improve the precision and accuracy of inspection, life is preferably served It produces, it is extremely urgent to make the more reasonable method of inspection.
Summary of the invention
Present invention aims at make more reasonable K2The measuring method of O content improves the precision of inspection and accurate Degree, preferably serves production.
In order to achieve the above objectives, as follows using technical solution:
K in potassium bichromate production2The measuring method of O content, comprising the following steps:
1) it removes chromium: taking potassium bichromate reaction solution V to be measured, in acid condition plus Cr VI is all reduced to three by reducing agent Valence chromium adds alkali neutralization to solution to be in neutrality, and 1-2h, filtration washing to no K are kept the temperature at a temperature of 90-100 DEG C+Until, collection is washed Wash liquid；
2) potassium tetraphenylborate precipitating generates: gained cleaning solution being heated to boiling, tetraphenylboron sodium is added dropwise under stirring condition Solution is precipitated to potassium tetraphenylborate is generated, cooling and standings；
3) step 2 gained coolant liquid precipitating transfer: is transferred to the G to dry to constant weight in 120 DEG C4In glass sand core funnel It filters, gained precipitating is washed dropping liquid with potassium tetraphenylborate and washed, and the W that dries to constant weight finally is placed in drying box；
4)K2O content is calculated as follows:
A=0.1314 × W × 1000/V；
Wherein, A:K2O content, g/L；W: dry weight, g are precipitated obtained by step 3；V: potassium bichromate reaction solution to be measured, L.
According to the above scheme, determine that Cr VI is all reduced to three using with diphenylcarbazide indicator inspection in step 1 Valence chromium.
According to the above scheme, it is mixed using sodium tetraphenylborate solution with a small amount of cleaning solution tail washings in step 1, no white precipitate generates Determine in filtering gained precipitating there is no K+。
The present invention has the beneficial effect that compared with the existing technology:
Pre-treatment uses conventional method, is measured after processing using the method for potassium chloride, it was demonstrated that is feasible, operation Method is simple compared with conventional method, as a result favorable reproducibility, and accuracy is high, almost the same with notional result, is potassium bichromate system Cr6 +/K+Balance provides foundation.
Specific embodiment
Following embodiment further illustrates technical solution of the present invention, but not as limiting the scope of the invention.
Embodiment 1
Weighing 50g, (the quasi- benchmark potassium bichromate to 0.0001g) adds suitable quantity of water in 250ml beaker, in heating on electric furnace Dissolution.It is transferred to after cooling in 250ml volumetric flask, is diluted with water to scale, shaken up, at this time K2O content about 63.9g/L.
Take 25.00ml in 4 first, second, third, fourth 250ml beakers respectively.Respectively plus 10ml hydrochloric acid (1+1) and appropriate second Alcohol and water is placed in 100 DEG C of water-baths and keeps the temperature 1-2 hours, until Cr6+Reduction thoroughly (is detected) with diphenylcarbazide indicator Afterwards, liquid feeding alkali adjusts solution to neutrality, keep the temperature 1 hour in boiling water bath, and with the filtering of quantitative filter paper at a slow speed, hot water is washed till no K+Until (being examined with sodium tetraphenylborate solution), diafiltration liquid are collected in 250ml beaker.
Wherein first, second difference traditionally carries out: it is different to add 1 drop methyl orange indicator respectively, with 10% acetic acid solution It adjusts to just taking on a red color, is heated to 60 DEG C and removes.10ml sodium tetraphenylborate solution is added dropwise under stiring, continues stirring 1 minute, Place after ten minutes, at 120 DEG C constant weight G4Glass pot filters, and it is heavy to be shifted with ethyl alcohol potassium tetraphenylborate saturated solution It forms sediment, and divides 3-4 washing to precipitate with 15ml, drain every time.Crucible is removed, washed once with 2ml dehydrated alcohol along crucible wall, is taken out It is dry.By G4Glass pot is dry to constant weight in 120 DEG C, is placed in drier after being cooled to room temperature and weighs.Public affairs traditionally Formula calculates:
First bottle, K2O content 58.31g/L
Second bottle, K2O content 55.28g/L
The third, fourth difference is separately heated to 70 DEG C or so according to the method for the present invention, and 10ml tetra- is added dropwise respectively under stiring Benzene boron sodium solution continues stirring 1 minute, and 20 DEG C are rapidly cooled in flowing water hereinafter, placing 10 minutes.With in advance at 120 DEG C The dry G to constant weight4Glass pot filters, and is precipitated in glass pot with the transfer of potassium tetraphenylborate cleaning solution liquid, continues with washing Liquid washing precipitating 12 times or so, each dosage about 5ml.By G4Glass pot is placed in 120 DEG C of drying boxes and dries to constant weight, and is placed in dry It weighs after being cooled to room temperature in dry device.It is calculated by above-mentioned formula:
Third sample K2O content 63.82g/L
Fourth sample K2O content 63.78g/L
The K measured according to this method2O content is averaged 63.8g/L, close to true value, from the point of view of preci-sion and accuracy, all It meets the requirements, reliable foundation can be provided for production.
And according to traditional detection method, parallel result absolute error reaches 3.03g/L, deviates true value, precision Testing requirements are not complyed with accuracy.

Claims (3)

1. K in potassium bichromate production2The measuring method of O content, it is characterised in that the following steps are included:
1) it removes chromium: taking potassium bichromate reaction solution V to be measured, in acid condition plus Cr VI is all reduced to trivalent by reducing agent Chromium adds alkali neutralization to solution to be in neutrality, and 1-2h, filtration washing to no K are kept the temperature at a temperature of 90-100 DEG C+Until, collect washing Liquid；
2) potassium tetraphenylborate precipitating generates: gained cleaning solution being heated to boiling, sodium tetraphenylborate solution is added dropwise under stirring condition It is precipitated to potassium tetraphenylborate is generated, cooling and standings；
3) precipitating transfer: step 2 gained coolant liquid is filtered, and gained precipitating is washed dropping liquid with potassium tetraphenylborate and washed, is finally placed in dry Dry to constant weight W in dry case；
4)K2O content is calculated as follows:
A=0.1314 × W × 1000/V；
Wherein, A:K2O content, g/L；W: dry weight, g are precipitated obtained by step 3；V: potassium bichromate reaction solution to be measured, L.
2. K in potassium bichromate production as described in claim 12The measuring method of O content, it is characterised in that use in step 1 with two Dinitrodiphenyl carbazide indicator inspection determines that Cr VI is all reduced to trivalent chromium.
3. K in potassium bichromate production as described in claim 12The measuring method of O content, it is characterised in that four benzene are used in step 1 Boron sodium solution is mixed with a small amount of cleaning solution tail washings, and no white precipitate, which generates, determines in filtering gained precipitating do not have K+。
CN201811258910.4A 2018-10-26 2018-10-26 K in potassium dichromate production2Method for measuring O content Active CN109211718B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113233507A (en) * 2021-06-15 2021-08-10 湖北振华化学股份有限公司 Method for preparing basic chromium sulfate from residual liquid in menadione production

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