CN109655545A - A kind of chromatographic analysis device and method preparing tert-butylamine for isobutene - Google Patents
A kind of chromatographic analysis device and method preparing tert-butylamine for isobutene Download PDFInfo
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- CN109655545A CN109655545A CN201811622096.XA CN201811622096A CN109655545A CN 109655545 A CN109655545 A CN 109655545A CN 201811622096 A CN201811622096 A CN 201811622096A CN 109655545 A CN109655545 A CN 109655545A
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- isobutene
- butylamine
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
- G01N30/8634—Peak quality criteria
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
- G01N2030/3084—Control of physical parameters of the fluid carrier of temperature ovens
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Abstract
The present invention relates to chromatographic analysis devices and method that tert-butylamine is prepared for isobutene, tert-butylamine field is prepared applied to isobutene, it is characterized in that entering gas chromatographic analysis using the gaseous mixture that improved static volumetric method prepares tert-butylamine and isobutene or isobutene and ammonia, the method for obtaining standard curve, this method include distribution circuit design and build and prepare gas and draw two steps of standard curve.The present invention has the advantages that the gas distribution platform built using the present apparatus, can make the more uniform of gas mixing, tert-butylamine and isobutene or isobutene and ammonia distribution simultaneously are realized, calibration efficiency is improved and accuracy, practical application value is bigger；Insulating box is added in static air distributing device, can be adjusted by temperature, keeps distribution application range wider；Sample introduction repeatability and experiment condition stability detrimental effect are avoided, while solving the problems, such as that usable floor area normalization method error is larger；The shortcomings that avoiding amine substance strong adsorption.
Description
Technical field
The present invention relates to a kind of chromatographic analysis devices and method that tert-butylamine is prepared for isobutene, are mainly used in isobutyl
Alkene prepares tert-butylamine field.
Background technique
Tert-butylamine is a kind of important organic intermediate, is widely used in synthesis medicine, pesticide, dyestuff colorant, rubber and promotees
Into agent and chemical reagent, the rubber accelerator N- tert-butyl -2-[4-morpholinodithio time sulphur dominated especially as global environment-friendly novel
The primary raw material of amide (NS) is paid attention to by domestic industry.Preparing the ideal route of tert-butylamine is directly to be reacted by alkene with ammonia
Synthesize tert-butylamine.
Isobutene direct aminatin method raw material sources are easy, and price is low, good reaction selectivity, are a kind of atom warps for having development potentiality
Help cleaning procedure, has become tert-butylamine synthesis field hottest point technology since the 1980s.Isobutene aminating method has product
The advantages that purity is high, by-product are few, but reaction technology difficulty is big under high temperature, condition of high voltage, and conversion ratio is not high, mostly on 15% left side
The right side, needs a large amount of Matter Transfer to utilize, and energy consumption is higher.Since isobutene conversion is low, a large amount of material needs to recycle again
Utilize, accurately calculating for conversion ratio is particularly important, while the design of knockout tower to conversion ratio and selectivity accuracy have it is higher
It is required that.
Currently, the domestic analysis method to isobutene direct aminatin method production tert-butylamine introduce it is less.In open report
The problem of what is used is area normalization method, and this method is easy, quick, but evaluated error is larger, influences measurement result, is unfavorable for
The industrial use of the technique.Amine substance absorption is strong, causes traditional scaling method error larger.
The present invention prepares the tert-butylamine and isobutene or isobutene and ammonia of various concentration using improved static volumetric method
Gaseous mixture enters gas chromatographic analysis, obtains standard curve, avoids sample introduction repeatability and the unfavorable shadow of experiment condition stability
The shortcomings that ringing, avoiding amine substance strong adsorption, while solving the problems, such as that error is larger when usable floor area normalization method.
Summary of the invention
The present invention is provided to chromatographic analysis devices and method that isobutene prepares tert-butylamine, using improved static distribution
Method prepares tert-butylamine and isobutene or isobutene and the gaseous mixture of ammonia enters gas chromatographic analysis, obtains the side of standard curve
Method prepares the calibration of tert-butylamine for isobutene direct aminatin method, to obtain accurate conversion ratio and ammonia alkene ratio.It is above-mentioned to realize
The technical solution that purpose uses are as follows:
A kind of chromatographic analysis device preparing tert-butylamine for isobutene, the design and building structure of distribution pipeline are as follows:
Vacuum pump connects distribution tank through valve 2, and differential manometer is directly connected to distribution tank, air inlet and sample tap and connects through valve 1 and 3
In in distribution tank.Distribution tank is placed in incubator, and equipped with stirring.
It include: to prepare gas and drafting standard song using the analysis method that isobutene prepares the chromatographic analysis device of tert-butylamine
Line,
For the gaseous mixture for preparing different mol ratio, specific operation process is as follows:
1. insulating box keeps certain temperature, distribution tank stirring is opened.
2. repeatedly replacing the air in distribution tank using inert gas.
3. opening vacuum pump, vacuumizing makes distribution tank in negative pressure state, records the differential manometer registration H after vacuumizing, isobutyl
Alkene by gas supplementing opening be passed through it is a certain amount of after, record differential manometer registration H1, then pass to ammonia or tert-butylamine, record differential manometer registration
H2.The molar ratio of two kinds of mixtures are as follows:
Formula (1)
Note: pressure difference is converted into the expression of millimetres of mercury height
4. inert gas is slowly added to distribution tank by gas supplementing opening, and makes distribution tank in barotropic state.
5. being sampled from sample tap, into gas-chromatography.
6. being passed through various inlet amount or liquid inlet volume, a series of mixed gas of various concentrations is obtained, through gas Chromatographic Determination,
A series of not cospectral graphs and corresponding peak area are obtained, the standard drawn between molar ratio and peak area ratio is bent
Line obtains calibration curve formula:
1. isobutene and ammonia
Formula (2)
2. isobutene and tert-butylamine
Formula (3)
Note: M is molal quantity, S be peak area, a and c be slope, b and d is intercept
According to obtained chromatographic peak area is actually sampled, practical isobutene and ammonia molar ratio are calculated.
The distribution tank stirring, is magnetic agitation, mechanical stirring.
The vacuum pump is water circulating type vacuum pump, rotary-vane vaccum pump etc..
The pipe valve is check valve, ball valve, needle-valve etc..
The pressure difference is calculated as U-shaped differential manometer, digital display type differential manometer, high-precision pressure gauge etc.
The inert gas of the supplement is hydrogen, helium, argon gas, nitrogen.
At a certain temperature, temperature is at 0~100 DEG C for the insulating box.
Described to make distribution tank in barotropic state with inert gas, positive pressure is 0~1000mm millimetres of mercury.
The beneficial effects of the present invention are:
The present invention relates to gas or the mixture of low-boiling point liquid, the method for carrying out gas-chromatographic titer, advantages of the present invention exists
In: (1) gas distribution platform using the present apparatus built can make the more uniform of gas mixing, realize tert-butylamine and isobutene
Or the distribution simultaneously of isobutene and ammonia, it improves calibration efficiency and accuracy, practical application value is bigger；(2) static air distributing device
Middle addition insulating box, can be adjusted by temperature, keep distribution application range wider.(3) sample introduction repeatability and experiment condition are avoided
Stability detrimental effect, while solving the problems, such as that usable floor area normalization method error is larger.(4) amine substance absorption is avoided
The strong disadvantage of property.
Detailed description of the invention
The present invention will be further explained below with reference to the attached drawings.
Fig. 1 is distribution piping installation figure；
Fig. 2 is liquefied ammonia and isobutene standard curve；
Fig. 3 is isobutene and tert-butylamine standard curve.
Specific embodiment
The present invention is made combined with specific embodiments below and being further elaborated on, but the invention is not limited to following realities
Apply example.
One, isobutene and ammonia molar ratio
(1) it prepares gas and draws standard curve
For the gaseous mixture for preparing different mol ratio, according to distribution piping installation figure, specific operation process is as follows:
1. insulating box is kept for 30 degrees Celsius, distribution tank magnetic agitation is opened;
2. repeatedly replacing the air in distribution tank using hydrogen;
3. opening vacuum pump, vacuumizing makes distribution tank in negative pressure state, record vacuumize after digital display type differential manometer registration H, it is different
Butylene by gas supplementing opening be passed through it is a certain amount of after, record digital display type differential manometer registration H1, then pass to ammonia, record digital display type differential manometer
Registration H2.Formula 1 is substituted into, obtains isobutene and ammonia molar ratio, (note: pressure difference registration is converted into millimetres of mercury altimeter
Show);
4. hydrogen is slowly added to distribution tank by gas supplementing opening, and makes distribution tank in barotropic state;
5. being sampled from sample tap, into gas-chromatography;
6. obtaining a series of mixed gas of various concentrations, data such as table 1 by the difference of air inflow:
1 ammonia of table and isobutene distribution data
Through gas Chromatographic Determination, a series of not cospectral graphs and corresponding peak area are obtained, draws molar ratio and peak face
Standard curve between product ratio.
(2) isobutene and ammonia molar ratio
According to the standard curve that liquefied ammonia and isobutene standard curve obtain, ammonia and isobutene molar ratio formula can be obtained such as
Under:
According to obtained chromatographic peak area is actually sampled, practical isobutene and ammonia molar ratio are calculated.
Two, isobutene and tert-butylamine molar ratio
(1) it prepares gas and draws standard curve
For the gaseous mixture for preparing different mol ratio, with reference to the accompanying drawings 1, specific operation process is as follows:
1. insulating box is kept for 30 degrees Celsius, distribution tank magnetic agitation is opened.
2. repeatedly replacing the air in distribution tank using hydrogen.
3. opening vacuum pump, vacuumizing makes distribution tank in negative pressure state, records the digital display type differential manometer registration after vacuumizing
H3, isobutene by gas supplementing opening be passed through it is a certain amount of after, record digital display type differential manometer registration H4, then pass to tert-butylamine, record digital display
Formula differential manometer registration H5.Formula 1 is substituted into, isobutene and ammonia molar ratio are obtained.(note: pressure difference registration is converted into millimetres of mercury
Height indicates)
4. hydrogen is slowly added to distribution tank by gas supplementing opening, and makes distribution tank in barotropic state.
5. being sampled from sample tap, into gas-chromatography.
6. obtaining a series of mixed gas of various concentrations, data such as table 2 by the difference of air inflow:
2 tert-butylamine of table and isobutene distribution data
Through gas Chromatographic Determination, a series of not cospectral graphs and corresponding peak area are obtained, draws molar ratio and peak face
Standard curve between product ratio.
(2) isobutene and tert-butylamine molar ratio
According to the standard curve that tert-butylamine and isobutene standard curve obtain, ammonia and isobutene molar ratio formula can be obtained such as
Under:
According to obtained chromatographic peak area is actually sampled, practical isobutene and tert-butylamine molar ratio are calculated.Above to the present invention
Specific implementation be described in detail, but be intended only as an example, the present invention is not restricted to described above specific
Case study on implementation, also within protection scope of the present invention to the equivalent modifications that carry out of the present invention.
Claims (10)
1. a kind of chromatographic analysis device for preparing tert-butylamine for isobutene, which is characterized in that including distribution tank, the distribution tank
By the connection of valve 2 on vacuum pump, it is also connected with differential manometer in distribution tank, is provided with valve on the air inlet of the distribution tank
1, valve 3 is provided on the sample tap of distribution tank, and the distribution tank is placed in incubator, configured with stirring dress in distribution tank
It sets.
2. the chromatographic analysis device of tert-butylamine is prepared for isobutene as described in claim 1, which is characterized in that the distribution
Agitating device in tank is magnetic agitation or mechanical stirring.
3. the chromatographic analysis device of tert-butylamine is prepared for isobutene as described in claim 1, which is characterized in that the vacuum
Pump is water circulating type vacuum pump or rotary-vane vaccum pump.
4. the chromatographic analysis device of tert-butylamine is prepared for isobutene as described in claim 1, which is characterized in that the vacuum
Valve is check valve, ball valve or needle-valve.
5. the chromatographic analysis device of tert-butylamine is prepared for isobutene as described in claim 1, which is characterized in that the pressure difference
It is calculated as U-shaped differential manometer, digital display type differential manometer or high-precision pressure gauge.
6. such as the analysis method using device described in claim 1, which comprises the following steps:
(1) gas is configured；
(2) standard curve is drawn.
7. analysis method as claimed in claim 6, which is characterized in that be the gaseous mixture for preparing different mol ratio, according to right
It is required that device described in 1, the step (1) the following steps are included:
1. insulating box keeps certain temperature, distribution tank stirring is opened；
2. repeatedly replacing the air in distribution tank using inert gas；
3. opening vacuum pump, vacuumizing makes distribution tank in negative pressure state, record vacuumize after differential manometer registration H, isobutene by
Gas supplementing opening be passed through it is a certain amount of after, record differential manometer registration H1, then pass to ammonia or tert-butylamine, record differential manometer registration H2；
The molar ratio of two kinds of mixtures are as follows:
Formula (1)
Wherein, pressure difference is converted into the expression of millimetres of mercury height；
4. inert gas is slowly added to distribution tank by gas supplementing opening, and makes distribution tank in barotropic state；
5. being sampled from sample tap, into gas-chromatography.
8. analysis method as claimed in claim 6, which is characterized in that the specific steps of step (2) are as follows: be passed through various inlet amount
Or liquid inlet volume, a series of mixed gas of various concentrations is obtained, through gas Chromatographic Determination, obtains a series of not cospectral graphs and therewith
Corresponding peak area draws the standard curve between molar ratio and peak area ratio, obtains calibration curve formula:
Isobutene and ammonia
Formula (2)
Isobutene and tert-butylamine
Formula (3)
Wherein, M is molal quantity, S be peak area, a and c be slope, b and d is intercept；
According to obtained chromatographic peak area is actually sampled, practical isobutene and ammonia molar ratio are calculated.
9. the analysis method as described in claim 6-8 any claim, it is characterised in that: the inert gas be hydrogen,
Helium, argon gas, nitrogen, the calorstat temperature is between 0~100 DEG C.
10. the analysis method as described in claim 6-8 any claim, it is characterised in that: make distribution tank with inert gas
In barotropic state, positive pressure is 0~1000mm millimetres of mercury.
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| CN201811622096.XA CN109655545A (en) | 2018-12-28 | 2018-12-28 | A kind of chromatographic analysis device and method preparing tert-butylamine for isobutene |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110988241A (en) * | 2019-12-16 | 2020-04-10 | 湖南九典制药股份有限公司 | Method for detecting and separating related substances in bambuterol |
| CN111289676A (en) * | 2020-01-20 | 2020-06-16 | 南京林业大学 | Method for detecting residual tert-butylamine in terbutaline sulfate bulk drug |
| CN111624280A (en) * | 2020-06-10 | 2020-09-04 | 郑州安诺科学仪器有限公司 | Device and method for automatically preparing gas standard curve |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN111289676A (en) * | 2020-01-20 | 2020-06-16 | 南京林业大学 | Method for detecting residual tert-butylamine in terbutaline sulfate bulk drug |
| CN111624280A (en) * | 2020-06-10 | 2020-09-04 | 郑州安诺科学仪器有限公司 | Device and method for automatically preparing gas standard curve |
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Application publication date: 20190419 |