CN101975838B - Method for measuring contents of total acid, sulfuric acid and formic acid in trioxymethylene polymerization reactor - Google Patents
Method for measuring contents of total acid, sulfuric acid and formic acid in trioxymethylene polymerization reactor Download PDFInfo
- Publication number
- CN101975838B CN101975838B CN201010287033A CN201010287033A CN101975838B CN 101975838 B CN101975838 B CN 101975838B CN 201010287033 A CN201010287033 A CN 201010287033A CN 201010287033 A CN201010287033 A CN 201010287033A CN 101975838 B CN101975838 B CN 101975838B
- Authority
- CN
- China
- Prior art keywords
- acid
- content
- sulfuric acid
- total
- ferrous sulfate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 78
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000002253 acid Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 27
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 235000019253 formic acid Nutrition 0.000 title claims abstract description 24
- BGJSXRVXTHVRSN-UHFFFAOYSA-N 1,3,5-trioxane Chemical group C1OCOCO1 BGJSXRVXTHVRSN-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 238000006116 polymerization reaction Methods 0.000 title abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 238000004448 titration Methods 0.000 claims description 23
- 239000011790 ferrous sulphate Substances 0.000 claims description 16
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 16
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 15
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 13
- 238000003556 assay Methods 0.000 claims description 9
- 229920000642 polymer Polymers 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000005259 measurement Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 3
- 238000009966 trimming Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- -1 sulfate radical Chemical class 0.000 description 2
- 241000282693 Cercopithecidae Species 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for measuring contents of total acid, sulfuric acid and formic acid in a trioxymethylene polymerization reactor. The method quantitatively analyzes the influence of each component in the reactor on the total acid measurement value during measuring the total acid, and eliminates the influence by adopting a correcting method so as to improve the measurement accuracy of the total acid. According to different physical and chemical properties of the sulfuric acid and the formic acid, a method for measuring the sulfuric acid and the formic acid respectively is established, the method is simple and feasible, and accurate measurement of the sulfuric acid content and the formic acid content becomes possible.
Description
Technical field
The present invention relates to a kind of content assaying method of acid, particularly relate to the assay method of total acid, sulfuric acid and formic acid content in a kind of trioxymethylene polymer reactor.
Background technology
In the trioxymethylene reactor, complicated component contains water, compositions such as sulfuric acid, formic acid, sulfate, methyl alcohol, dimethoxym ethane.The accurate control of catalyst sulfuric acid content is the key of production process, but all is adopt to add barium chloride to measure the amount that the growing amount of barium sulphate is confirmed sulfate radical all the time; The amount of sulfate radical is regarded as the amount of sulfuric acid; This analytical approach has also counted the content of sulfuric acid with the amount of sulfate in the system, causes measurement result higher, and the present invention is on this basis; A kind of new method is proposed, with the content of sulfuric acid, formic acid and total acid in the accurate measurement reactor.
Summary of the invention
The assay method that the purpose of this invention is to provide total acid, sulfuric acid and formic acid content in a kind of trioxymethylene polymer reactor.
For achieving the above object, technical scheme of the present invention provides the assay method of total acid, sulfuric acid and formic acid content in a kind of trioxymethylene polymer reactor, may further comprise the steps:
(1) content of total acid in the assaying reaction device: the content of total acid in the assaying reaction device behind the calibrated ferrous sulfate of employing NaOH titrimetry;
(2) sulfuric acid and the formic acid in the heating separate reactor is measured the wherein content of sulfuric acid behind the calibrated ferrous sulfate;
(3) total acid content deducts sulfuric acid content and obtains formic acid content.
Preferably adopt the NaOH titrimetry when measuring total acid content in the assay method of the present invention, said step (1).The method is simple and the result is accurate.When measuring, for other components in the elimination system are proofreaied and correct the influence of total acidity test; Trimming process is: in the trioxymethylene synthesis reactor; The main existence is ferrous sulfate, and this part salt can generate a certain amount of ferrous hydroxide measuring in the process of total acid and sulfuric acid with the NaOH standard titration solution; React away the NaOH of a part, cause measuring the higher of result.This method adopts and quantitatively adds from the method for the different content ferrous sulfate of 1500PPM～30000PPM; Adopt the NaOH volumetric soiutions of 0.5mol/L to adopt autotitrator to come the sulfuric acid and the formic acid biased sample of titration known content; Test findings proves, is constant in the process of titration total acid, causing result's numerical value bigger than normal greater than the ferrous sulfate more than the 3000PPM.This constant value is the corrected value of the total acid under the volumetric soiutions of the NaOH that adopts 0.5mol/L and these two conditions of method that autotitrator configures.The mensuration result of total acid deducts this corrected value and is total acid numerical value accurately.For trioxymethylene reactor, the content of its ferrous ion is generally all between 300PPM～20000PPM.Be included within the trial stretch of this corrected value.
Assay method of the present invention; Sulfuric acid adopts normal titration method can't accomplish the two is accurately separated with the separation method of formic acid in the said step (2), and this method is utilized the two volatile different and different with the azeotropic point of the potpourri of water when heating of sulfuric acid and formic acid, reaches formic acid and is heated to the phenomenon that uniform temperature promptly begins decomposes; Choose a reasonable temperature (like 110 degree; Sample size should not be too big, generally chooses 2～2.5 grams) the insulation certain hour, guarantee that formic acid volatilization decomposition finishes in the sample; Like this in this individual system, and the ferrous sulfate that sulfuric acid and influence are measured is still stayed in the sample.And ferrous salt is not varied to molysite in this process.
Identical NaOH standard titration solution and identical automatic titration impose a condition when adopting with the mensuration total acid when measuring sulfuric acid content in the assay method of the present invention, said step (2).In only containing the titration system of sulfuric acid; Ferrous salt is different to the influence of titration results and total acidity test result's influence value; The same content range of the ferrous sulfate when measuring the total acid corrected value and the identical titrator of adopting is provided with condition; Also obtain the constant influence value that a ferrous sulphate salt pair has only the titration system of sulfuric acid, the corrected value of this corrected value during than total acidity test is little.This is because contain the reason of formic acid in the total acid.The sulfuric acid content that determines is deducted this corrected value, be real sulfuric acid and measure the result.
Technique scheme has following advantage: through the mensuration process was divided into for three steps; Every pacing is regularly proofreaied and correct accurately; Guaranteed the accurate mensuration of various acid contents in the trioxymethylene polymer reactor, the content of each material in the more accurate controlling reactor effectively.
Embodiment
Below in conjunction with embodiment, specific embodiments of the invention describes in further detail.Following examples are used to explain the present invention, but are not used for limiting scope of the present invention.
1, the mensuration of total acid: get 40ML distilled water; Zero clearing on ten thousand/balance; With ST draw 2 gram samples (wherein sample be immediately from trioxymethylene polymer reactor R210 airtight insulation fetch, draw with suction pipe), splash in the water of firm zero clearing; Write down concrete weight M, (the method is taken the total acid corrected value that determines into account by the method that has configured with autotitrator then; Trimming process is that the fixed value of ferrous sulphate salt pair titration results influence is removed in computing formula for 0.20 milliliter in advance) the beginning titration; What titrant used is the NaOH standard titration solution of 0.5mol/L; Weight input titrator with sample; Titration finishes, and instrument is quoted the total acid result of overcorrect automatically.
2, the mensuration of sulfuric acid: get the sample about 2 grams with monkey; Write down weight M, put into and rise to the electric furnace that temperature (110 degree) is set, insulation finishes to the time (20 minutes) is set; Take out; Cooling all is transferred to titration cup with the residue in the crucible, and (the method is taken the sulfuric acid corrected value that determines into account by the method that has configured with autotitrator then; Trimming process is that the fixed value of ferrous sulphate salt pair titration results influence is removed in computing formula for 0.18 milliliter in advance) the beginning titration, what titrant used is the NaOH standard titration solution of 0.5mol/L.With the weight input titrator of sample, titration finishes, and instrument is quoted the sulfuric acid result of overcorrect automatically.
3, total acid content deducts sulfuric acid content and promptly obtains formic acid content.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from know-why of the present invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (2)
1. the assay method of the interior total acid of trioxymethylene polymer reactor, sulfuric acid and formic acid content is characterized in that, may further comprise the steps:
(1) content of total acid in the assaying reaction device: the content of total acid in the assaying reaction device behind the calibrated ferrous sulfate of employing NaOH titrimetry; The method of said correction ferrous sulfate is: in the sulfuric acid of known content and formic acid biased sample, quantitatively add from the ferrous sulfate of the different content of 1500PPM～30000PPM; Adopt the NaOH volumetric soiutions of 0.5mol/L; Adopt autotitrator to come the titration total acid, obtain the corrected value of the total acid under the equal conditions;
(2) sulfuric acid and the formic acid in the heating separate reactor is measured the wherein content of sulfuric acid behind the calibrated ferrous sulfate; The method of said correction ferrous sulfate is: in the sulfuric acid sample of known content, quantitatively add from the ferrous sulfate of the different content of 1500PPM～30000PPM; Adopt the NaOH volumetric soiutions of 0.5mol/L; Adopt autotitrator to come titration sulfuric acid, obtain the corrected value of the sulfuric acid under the equal conditions;
(3) total acid content deducts sulfuric acid content and obtains formic acid content.
2. assay method as claimed in claim 1 is characterized in that, heating refers to and is heated to 110 degree in the said step (2), is incubated 20 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010287033A CN101975838B (en) | 2010-09-16 | 2010-09-16 | Method for measuring contents of total acid, sulfuric acid and formic acid in trioxymethylene polymerization reactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010287033A CN101975838B (en) | 2010-09-16 | 2010-09-16 | Method for measuring contents of total acid, sulfuric acid and formic acid in trioxymethylene polymerization reactor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101975838A CN101975838A (en) | 2011-02-16 |
| CN101975838B true CN101975838B (en) | 2012-10-03 |
Family
ID=43575740
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010287033A Expired - Fee Related CN101975838B (en) | 2010-09-16 | 2010-09-16 | Method for measuring contents of total acid, sulfuric acid and formic acid in trioxymethylene polymerization reactor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101975838B (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1136812A (en) * | 1993-12-06 | 1996-11-27 | 赫希斯特人造丝公司 | Process for production of trioxane from formaldehyde |
-
2010
- 2010-09-16 CN CN201010287033A patent/CN101975838B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1136812A (en) * | 1993-12-06 | 1996-11-27 | 赫希斯特人造丝公司 | Process for production of trioxane from formaldehyde |
Non-Patent Citations (2)
| Title |
|---|
| 于凤兰.多聚甲醛含量的快速测定.《天津化工》.1996,(第1期),36-37、27. * |
| 季德岩.甲醛水溶液中甲酸和硫酸的分别测定.《化学世界》.1984,(第9期),333-334. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101975838A (en) | 2011-02-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103267754B (en) | The method of macroelement and arsenic, tin, antimony trace element in quantitative measurement carbon steel or low alloy steel | |
| CN104897766B (en) | The bearing calibration of trace element in a kind of use Isotope Dilution Mass Spectrometry sample | |
| CN104198484A (en) | Method for testing fluorine content in solution | |
| CN102426168A (en) | Method for measuring free lead in lead-acid battery green plate sample | |
| ATE554400T1 (en) | METHOD FOR MAKING A FIBER CURRENT SENSOR WITH INHERENT FARADAY EFFECT TEMPERATURE COMPENSATION | |
| CN110642964A (en) | Epoxy functional rubber crosslinked elastomer capable of being repeatedly processed and preparation method thereof | |
| CN109439812B (en) | Method for measuring high-slag discharge amount and defoaming blast furnace slag | |
| CN109490397B (en) | Method for rapidly determining SO3 content in coal ash by adding activated carbon | |
| CN101975838B (en) | Method for measuring contents of total acid, sulfuric acid and formic acid in trioxymethylene polymerization reactor | |
| CN102590182A (en) | Detection method for micro constituents in glass | |
| WO2021068186A1 (en) | Preparation method for pva fiber | |
| CN104422685A (en) | Method for determining content of metal aluminum in ladle slag modifying agent | |
| CN106908553A (en) | A kind of method for improving indapamide tablets stability in an acidic solution | |
| CN105823536B (en) | The method that marker method measures cigarette overlapping glue resin added | |
| CN103822850A (en) | Method for determination of content of calcium metal in calcium-series cored wires | |
| CN112362653B (en) | Method for detecting low chlorine content of photoinitiator | |
| CN103063665B (en) | Determination method for content of boron trifluoride in formaldehyde copolymerization catalyst | |
| CN105463642B (en) | Dead zone length automatic testing method in the control of drawing frame autoleveller | |
| CN107677765A (en) | A kind of method for deriving Production by Catalytic Combustion Process measure hydroxylamine salt organic residue based on TOC | |
| CN104090000B (en) | A kind of Velcade important intermediate content assaying method and application thereof | |
| CN208757283U (en) | A kind of acid-base accommodation device | |
| CN103399011A (en) | Measuring method of content of cyanoacetic acid product | |
| CN105617894A (en) | Full-automatic high-precision dissolving system | |
| CN102688723A (en) | Charging metering device for reaction kettle | |
| CN111175252A (en) | Method for detecting butanone oxime content by Abbe refractometer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20121003 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |