CN101545890B - Method for on-line measurement of sec-butyl alcohol content in butylene hydration product - Google Patents
Method for on-line measurement of sec-butyl alcohol content in butylene hydration product Download PDFInfo
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- CN101545890B CN101545890B CN2009100223117A CN200910022311A CN101545890B CN 101545890 B CN101545890 B CN 101545890B CN 2009100223117 A CN2009100223117 A CN 2009100223117A CN 200910022311 A CN200910022311 A CN 200910022311A CN 101545890 B CN101545890 B CN 101545890B
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- butyl alcohol
- butylene hydration
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Abstract
The invention provides a method and equipment for on-line measurement of sec-butyl alcohol content in a butylene hydration product. The method comprises the following steps: the butylene hydration product enters a separation tank through the outlet of a reactor for steam-liquid separation, a steam phase is discharged from a system through the top of the separation tank after backpressure through a backpressure valve, and a liquid phase is pumped into a liquid sampling valve through a measuring pump after being filtered and is analyzed through a chromatograph analyzing system to obtain the content of sec-butyl alcohol in the butylene hydration product. The invention adopts an on-line analyzing system, thereby the sampling process is simplified, the tedious steps of the prior sampling method are greatly reduced, and the artificial errors of analysis are reduced. The liquid sampling valve is used for sampling, and an external standard method is adopted to analyze the concentration of the butylene hydration product, thereby analyzed quantification in every time is accurate, and an analysis result really and reliably responses the concentration of the butylene hydration product.
Description
Technical field
The invention belongs to the petrochemical technology field, relate to the method and apparatus of sec-butyl alcohol content in a kind of on-line determination butylene hydration product.
Background technology
Utilize the technological process of n-butene and water reacted sec-butyl alcohol to be: raw material n-butene and water from head tank after mixer mixing; Enter into primary heater and carry out preheating; Under certain temperature and pressure, get into the reactor internal reaction and generate sec-butyl alcohol then, unreacted butylene, water and product sec-butyl alcohol are behind counterbalance valve; Outflow reactor under atmospheric pressure state, the mensuration of sec-butyl alcohol content is generally determined off-line in the outlet material.Concrete operations are: take by weighing a certain amount of deionized water, will react the outlet material water and absorb, a small amount of butylene is with all sec-butyl alcohol and unreacted water are dissolved in the water; Use gas chromatographic analysis then; With the packed column is chromatographic column, adopts internal standard method, obtains sec-butyl alcohol content in the water.This this method mainly is gain in weight poor that absorbs water according to the material quantity that gets into consersion unit and reaction back, utilizes stratographic analysis, measures the content of hydration reaction product sec-butyl alcohol.This method need write down the sampling time section accurately when sampling, it is poor that weighing absorbs the weightening finish of water before and after sampling, then according to the inlet amount and the sampling quantity of record, specifically calculates the content of sec-butyl alcohol.This method intermediate link is many, complex steps, and personal error is big, thereby has influenced accuracy and the stability measured.
Summary of the invention
The objective of the invention is in order to overcome the deficiency of prior art, the method for sec-butyl alcohol content in a kind of on-line determination butylene hydration reaction product is provided.
Another object of the present invention provides a kind of equipment of realizing sec-butyl alcohol content in the on-line determination butylene hydration reaction product.
The method of sec-butyl alcohol content in the on-line determination butylene hydration reaction product of the present invention; Be butylene hydration product to be got into separating tank carry out vapor-liquid separation; Vapour phase is discharged system from the separating tank top after the counterbalance valve back pressure; Liquid phase gets into chromatographic analysis system by the liquid sampling valve after filtering and analyzes, and obtains the content of sec-butyl alcohol in the butylene hydration reaction product.
Chromatographiccondition of the present invention is: adopt external standard method, chromatographic column is 10% polyglycol packed column, and column temperature is 60～80 ℃, and vapourizing temperature is that 120～140 ℃, detected temperatures are that 140～160 ℃, sample size are 5～10uL.
The equipment of sec-butyl alcohol content comprises knockout drum in the on-line determination butylene hydration reaction product of the present invention, and the top of separating tank is provided with vapour phase and goes out system, and the bottom of knockout drum is provided with liquid phase and goes out system.Wherein vapour phase goes out system and comprises stop valve and counterbalance valve successively; Liquid phase goes out system and comprises liquid level sighting tube, filtrator, fixed displacement pump, liquid sampling valve and vapour phase chromatograph successively.
The butylene hydration reaction product directly gets into knockout drum from the outlet of reactor, and the pressure of control knockout drum is below 0.15Mpa, and temperature is controlled to be 20～28 ℃, and the gas-liquid of butylene hydration reaction product is separated; Vapour phase goes out through gas-liquid separation tank top vapour phase after the counterbalance valve back pressure of system to discharge system from the separating tank top, and guarantees that the gas-liquid separation tank level provides an environment stably.After liquid phase goes out the filtrator filtration of system from the knockout drum bottom liquid phases; By the produced quantity of fixed displacement pump according to the butylene hydration reaction product, sample is squeezed into quantifying ring, get into gas chromatograph by the liquid sampling valve again; To each component concentration in the butylene hydration mixed reaction product, make accurate analysis.
The present invention compared with prior art has the following advantages:
1, the present invention is employed in line analysis technology and corresponding apparatus, and sampling process is oversimplified, and has significantly reduced the loaded down with trivial details step of original method of sampling, has reduced the personal error of analyzing.
2, the present invention uses liquid sampling valve sample introduction, adopts external standard method to analyze butylene hydration product concentration, makes the quantitatively accurate of each analysis, the reaction butylene hydration product concentration that analysis result is more true and reliable.
3, the present invention can promptly and accurately obtain analysis result when needs are known the device working order, and operation has stronger directive function to device.
Description of drawings
Fig. 1 is the equipment and the process flow diagram of sec-butyl alcohol content in the on-line determination butylene hydration product of the present invention.Code name is following among the figure:
1---tensimeter 2---stop valve 3---counterbalance valve
4---knockout drum 5---liquid level sighting tube 6---filtrators
7---fixed displacement pump 8---liquid sampling valve 9---gas chromatographs
Embodiment
The equipment of sec-butyl alcohol content in the on-line determination butylene hydration reaction product:
This equipment comprises a knockout drum 4, and the top of knockout drum is provided with gas phase and goes out system, and the bottom of knockout drum is provided with liquid phase and goes out system.Wherein gas phase goes out system and comprises stop valve 2 and counterbalance valve 3 successively.For the ease of observing, the vapour phase at the top of separating tank goes out system tensimeter 1 also is installed, and comes the pressure in the display separation jar, so that through counterbalance valve regulating tank internal pressure.Liquid phase goes out system and comprises liquid level sighting tube 5, filtrator 6, fixed displacement pump 7, liquid sampling valve 8 and vapour phase chromatograph 9 successively.
The method of sec-butyl alcohol content in the on-line determination butylene hydration reaction product: butylene hydration product is directly got into knockout drum 4 from reactor outlet carry out vapor-liquid separation; Vapour phase is discharged system from the separating tank top after counterbalance valve 3 back pressures; Liquid phase is after filtrator filters; Squeeze into liquid sampling valve 8 by fixed displacement pump 7, get into chromatographic analysis system by liquid sampling valve 8 again and analyze, obtain the content of sec-butyl alcohol in the butylene hydration reaction product.Specific operation process is following:
1, draws calibration curve
Preparation contains five groups of the standard models of butylene hydration mix products (sec-butyl alcohol), gets into the analysis of chromatograph sample introduction through six-way injection valve.Be calculated as follows correction factor:
In the formula:
R
f-correction factor
C
Mark-concentration, m
A
MarkThe area that-stratographic analysis obtains
Measure the correction factor of component, draw calibration curve.
2, on-line analysis flow process and condition
After the butylene hydration reaction product is come out from reactor, get into separating tank 4, the regulating tank internal pressure is below the 0.15Mpa, carries out gas-liquid separation, and gas phase (unreacted butylene) is through counterbalance valve 3 removal systems.Liquid phase keeps liquid level at 8～12cm in separating tank 1.Liquid phase is through filtrator 6, and fixed displacement pump 7 gets into vapour phase chromatograph 9 by liquid sampling valve 8 and carries out gas chromatographic analysis.The control chromatographiccondition: hydrogen flame detector, polyglycol 10% chromatography packed column post, column temperature is 60～80 ℃, vapourizing temperature is that 120～140 ℃, detected temperatures are that 140～160 ℃, sample size are 5～10uL.
3, analysis result
Be calculated as follows the content of sec-butyl alcohol in the butylene hydration reaction product:
C＝AR
f
In the formula:
The content of product in the C-sample, m;
A-sample component chromatographic peak area;
R
f-constituent mass correction factor.
Claims (2)
1. the method for sec-butyl alcohol content in the on-line determination butylene hydration reaction product; Be the butylene hydration reaction product to be got into knockout drum carry out vapor-liquid separation; Vapour phase is discharged system from the gas-liquid separation tank top after the counterbalance valve back pressure; Liquid phase gets into gas chromatography system by the liquid sampling valve after filtering and analyzes, and obtains the content of sec-butyl alcohol in the butylene hydration reaction product; Analytical conditions for gas chromatography is: adopt external standard method, chromatographic column is 10% polyglycol packed column, and column temperature is 60～80 ℃, and vapourizing temperature is that 120～140 ℃, detected temperatures are that 140～160 ℃, sample size are 5～10uL.
2. the method for sec-butyl alcohol content in the on-line determination butylene hydration reaction product according to claim 1, it is characterized in that: the pressure control of said separating tank is below 0.15Mpa, and temperature is controlled to be 20～28 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2009100223117A CN101545890B (en) | 2009-04-16 | 2009-04-16 | Method for on-line measurement of sec-butyl alcohol content in butylene hydration product |
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| CN2009100223117A CN101545890B (en) | 2009-04-16 | 2009-04-16 | Method for on-line measurement of sec-butyl alcohol content in butylene hydration product |
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| Publication Number | Publication Date |
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| CN101545890A CN101545890A (en) | 2009-09-30 |
| CN101545890B true CN101545890B (en) | 2012-04-25 |
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| CN2009100223117A Expired - Fee Related CN101545890B (en) | 2009-04-16 | 2009-04-16 | Method for on-line measurement of sec-butyl alcohol content in butylene hydration product |
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| CN110187017A (en) * | 2019-05-09 | 2019-08-30 | 中触媒新材料股份有限公司 | A kind of propylene oxide on-line period device and method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5499531A (en) * | 1995-03-17 | 1996-03-19 | The Mitre Corporation | System and method for determining volatile constituents, vapor pressure and vapor emissions of liquids |
| CN1962576A (en) * | 2005-11-11 | 2007-05-16 | 中国石油化工股份有限公司 | Method for producing propylene ethane by carbon-containing olefin catalytic cracking |
| CN101395110A (en) * | 2006-03-02 | 2009-03-25 | 出光兴产株式会社 | Reactor for preparing sec-butyl alcohol |
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2009
- 2009-04-16 CN CN2009100223117A patent/CN101545890B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5499531A (en) * | 1995-03-17 | 1996-03-19 | The Mitre Corporation | System and method for determining volatile constituents, vapor pressure and vapor emissions of liquids |
| CN1962576A (en) * | 2005-11-11 | 2007-05-16 | 中国石油化工股份有限公司 | Method for producing propylene ethane by carbon-containing olefin catalytic cracking |
| CN101395110A (en) * | 2006-03-02 | 2009-03-25 | 出光兴产株式会社 | Reactor for preparing sec-butyl alcohol |
Non-Patent Citations (2)
| Title |
|---|
| 王凤霞 等.气相色谱法测定水-仲丁醇的含量.《山东化工》.2008,第37卷30-32. * |
| 陈小平 等.气相色谱法测定C4烃中的微量杂质.《石油化工》.2007,第36卷(第10期),1052-1055. * |
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