CN108459015A - A kind of detection method for producing silicone content in four unstripped gas of carbon after the ether of isooctane - Google Patents
A kind of detection method for producing silicone content in four unstripped gas of carbon after the ether of isooctane Download PDFInfo
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- CN108459015A CN108459015A CN201810418308.6A CN201810418308A CN108459015A CN 108459015 A CN108459015 A CN 108459015A CN 201810418308 A CN201810418308 A CN 201810418308A CN 108459015 A CN108459015 A CN 108459015A
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- ether
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- unstripped gas
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- 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
Abstract
The present invention provides the detection methods of silicone content in four unstripped gas of carbon after a kind of ether being used to produce isooctane.Detection method includes：(a) bright sulfur acid is added to the container, is sealed；(b) into container be added ether after four unstripped gas sample of carbon；(c) container is rocked so that four unstripped gas sample of carbon reacts in a reservoir after ether；(d) after reaction, it deflated, bled off pressure to container；(e) reaction product layer is taken, is diluted；Then, using ICP external standard methods, the silicone content in product is detected.Detection method indirectly can be detected the silicone content in unstripped gas by spectroscopic methodology, the expection of silicone content in the final isooctane product greatly improved, improve production efficiency；Meanwhile detection method step is easy, detection efficiency is high and testing result accuracy is high, section is reproducible, can accurately reflect that the silicone content in unstripped gas is horizontal.
Description
Technical field
The present invention relates to chemical spectrum detection fields, in particular to carbon four after a kind of ether for producing isooctane
The detection method of silicone content in unstripped gas.
Background technology
Currently, alkyl plant is the main technique for producing isooctane, the silicon after alkylation production ether used in carbon four contains
Amount will be transferred completely into isooctane finished product in process of production, and isooctane silicone content index is a very crucial index,
Silicone content index is once exceeded in unstripped gas, it will cause silicone content in finished product exceeded, the exceeded finished product of silicone content again be difficult into
Row handles and keeps silicone content up to standard in next step, brings certain difficulty to production, very big waste is caused to enterprise.Moreover, existing side
In method, the also not correlative study to the detection of the middle silicon of raw material.
In view of this, special propose the present invention.
Invention content
The first object of the present invention is to provide after a kind of ether for producing isooctane silicone content in four unstripped gas of carbon
Detection method, the detection method have many advantages, such as easy, efficiently, and testing result is accurate.
In order to realize that the above-mentioned purpose of the present invention, spy use following technical scheme：
A kind of detection method for producing silicone content in four unstripped gas of carbon after the ether of isooctane, the detection method include
Following steps：
(a) bright sulfur acid is added to the container, is sealed；
(b) into container be added ether after four unstripped gas sample of carbon；
(c) container is rocked so that four unstripped gas example reaction of carbon after ether；
(d) after reaction, it deflated, bled off pressure to container；
(e) reaction product layer is taken, is diluted；Then, using ICP external standard methods, the silicone content in product is examined
It surveys.
Preferably, in detection method of the present invention, the addition of bright sulfur acid is the 12~18% of container volume；
It is furthermore preferred that the addition of bright sulfur acid is the 15~17% of container volume.
Preferably, in detection method of the present invention, the step of four unstripped gas sample of carbon after ether is still further comprised
Suddenly.
Preferably, in detection method of the present invention, four unstripped gas sample of carbon includes the following steps after ether：
Sampler is connected to four unstripped gas sample storage tank of carbon after ether, after opening storage tank valve, discharge gas is to there is liquid
Then body collects liquid, four unstripped gas sample of carbon as after ether.
Preferably, in detection method of the present invention, the addition of four unstripped gas sample of carbon is container volume after ether
60~70%；
It is furthermore preferred that the addition of four unstripped gas sample of carbon is the 60~65% of container volume after ether.
Preferably, in detection method step (c) of the present invention, the time for rocking container is 1~5min；
It is furthermore preferred that in step (c), further include after rocking container, the step of placement that container is static.
Preferably, it is diluted to described in detection method step (e) of the present invention by product dilution to 30~50 times；
It is diluted to product dilution to 40~50 times it is furthermore preferred that stating.
Preferably, in detection method step (e) of the present invention, it is diluted to product with white oil.
Preferably, in detection method step (e) of the present invention, spectral conditions are：
Plasma flow 15~20L/min of amount, 0.5~1.5L/min of secondary air amount, atomizer throughput 0.1~
0.5L/min, 1300~1500W of power, 500~800r/min of pump speed, 15~30ml/min of oxygen, cryogenic temperature -10~-20
DEG C, 1~-1mm of quarter bend position.
Compared with prior art, beneficial effects of the present invention are：
Detection method indirectly can be detected the silicone content in unstripped gas by spectroscopic methodology, greatly improve
Final isooctane product in silicone content expection, improve production efficiency；
Meanwhile detection method step is easy, detection efficiency is high and testing result accuracy is high, section is reproducible,
It can accurately reflect that the silicone content in unstripped gas is horizontal.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described.
Fig. 1 is four raw material sampler structural schematic diagram of carbon after the ether provided in the specific embodiment of the invention；
Fig. 2 be the specific embodiment of the invention provided in deflation, bleed off pressure step apparatus structure schematic diagram；
Fig. 3 is the product sampling procedure apparatus structure schematic diagram provided in the specific embodiment of the invention.
Wherein, in Fig. 1, four feed line of carbon after 1- ethers, four raw material line sampling line of carbon after 2- ethers, 3- sample cocks, 4-
Double-ended needle, 5- pressure resistance glass sample containers；
In Fig. 2,1- syringe needles, the container of 2- sealings；
In Fig. 3,1- containers, 2- pipette, 3- products, 4- mixed materials.
Specific implementation mode
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
In view of in existing method, there is no the correlative study that silicone content in isooctane unstripped gas detects, spy of the present invention carries
The detection method for having supplied silicone content in a kind of isooctane unstripped gas, by easily and efficiently detecting step, to realize for original
Expect that the silicone content in gas is horizontal to accurately reflect, and then improves production efficiency.
Detection method specific steps provided by the present invention can refer to as follows：
(a) bright sulfur acid is added to the container, is sealed；
In this step, the addition of bright sulfur acid will preferably be controlled the 12~18% of container volume (calibration volume), example
It such as can be, but be not limited to 13,14,15,16 or 17% etc.；Preferably, the addition of bright sulfur acid be container volume 15~
17%；
The use of bright sulfur acid is mainly to play the role of catalytic action, and the alkene after ether in carbon four polymerize under sulfuric acid catalysis
To isooctane, the method for then recycling spectral detection is detected the silicone content in product isooctane, and then indirectly anti-
The silicone content reflected after ether in four raw material of carbon is horizontal.
Since four raw material of carbon exists in the form of gas (liquefied gas) after ether, thus impurity can not be carried out to it by spectrum
Ingredient (such as silicon etc.) detects；And it is silicon etc. included in four raw material of carbon after the ether for after its catalytic polymerization, participating in reaction is contaminated
Close object still can be contained in product (silicon impurities after the unreacted ether of minute quantity in four raw material of carbon will not with pure sulfuric acid reaction,
It thus still sweeps along after ether in four gas raw material of carbon, the accuracy of testing result can't be influenced).Thus, by for this
The detection of silicone content in portion of product, it will be able to obtain the contents level of the impurity such as silicon in raw material C4.
Meanwhile in this step, container used is pressure vessel；Due to after ether four compound of carbon be in the form of liquefied gas into
One step is added to the container, and reaction process is exothermic reaction, increases so as to cause vessel temp and interior pressure increases.Therefore, this hair
Container used is preferably heat-resistant pressure vessel in bright；
Further, for the ease of observing response process condition, container used is preferably pressure-resistant glass and takes in the present invention
Sample device.
(b) into container be added ether after four unstripped gas sample of carbon；
Further include the steps that sampling, referring to FIG. 1, this step includes before unstripped gas sample is added in this step：
One end of double-ended needle 4 is connected with four raw material line sampling line 2 of carbon after ether；
Then, sample cock 3 is opened, four unstripped gas of carbon is continued by being discharged in four feed line 1 of carbon after ether after ether
Discharge gas is to there is liquid (four raw material liquefied gas of carbon i.e. after ether)；
Then liquid, four raw material of carbon as after ether are collected by the pressure-resistant glass sample containers 5 being connect with the other end of double-ended needle 4
Gas sample product (that is, unstripped gas of the present invention be liquefied gas, using the liquefied gas of liquid condition as raw material, be not only convenient for raw material transfer and
Measurement, at the same be also beneficial to polymerisation effectively, the progress of scale, it is ensured that the accuracy of testing result).
Then, collected unstripped gas is added in the sealing container equipped with bright sulfur acid (preferably, can utilize double end
Collected unstripped gas is imported into reaction vessel by needle).
In this step, the addition of four unstripped gas sample of carbon is the 60~70% of container volume after ether, such as can be, but
It is not limited to 61,62,63,64,65,66,67,68 or 69% etc.；Preferably, the addition of four unstripped gas sample of carbon is after ether
The 60~65% of container volume；
Further, due to exothermic heat of reaction and C4 liquefied gas endothermic gasification volume expansions, in order to ensure in detection process
The total amount of safety, bright sulfur acid and unstripped gas should be controlled the 85% or less of container volume.
(c) container is rocked so that four unstripped gas sample of carbon reacts in a reservoir after ether；
After the completion of four unstripped gas of carbon is added after bright sulfur acid and ether, container is rocked so that the two comes into full contact with, carbon four after ether
Unstripped gas generates isooctane under the conditions of sulphuric acid catalysis；
Preferably, the time of vessel shaken is 1~5min, such as can be, but be not limited to 2,3 or 4min etc.；
Further, after by rocking so that raw material and sulfuric acid comes into full contact with, it may further include and shake in this step
The step of being stood after rolling so that four unstripped gas of carbon can fully carry out polymerisation after ether；
The time of standing preferably controls in 15~45min, such as can be, but be not limited to 20,25 or 30min etc.；
During standing, response situation in container is observed, dangerous generation is avoided.
(d) after reaction, it deflated, bled off pressure to container；
Referring to FIG. 2, after reaction, using syringe needle 1, the container 2 of sealing is subjected to gas and pressure discharges,
By do not carry out polymerisation, gasification after ether after four raw material liquefied gas of carbon be discharged.
(e) reaction product is taken, is diluted；Then, using ICP external standard methods, the silicone content in product is detected.
After in container without gas, without pressure, sealing cover is opened；Then, it takes out, is diluted from top by product；
Referring to FIG. 3, product sampling procedure is specific as follows：The product 3 on 1 upper layer of container is taken out with pipette 2, and lower layer
It is then mixed material 4；
Mixed material 4 is mainly the bright sulfur acid as catalyst, and other a small amount of products.
Preferably, it is by product dilution with white oil to 30~50 times, such as can is, but is not limited to white oil that product is dilute
It releases to 35,40 or 45 times etc..
Then, by the product after dilution by ICP (emission spectrum), and the inspection of silicone content is carried out by the way of external standard method
It surveys.
Further, standard sample equally will be also diluted before carrying out spectral detection with white oil, extension rate with wait for
It is identical to detect product.
Meanwhile the condition of emission spectrum is：Plasma flow 15~20L/min of amount, 0.5~1.5L/ of secondary air amount
Min, atomizer 0.1~0.5L/min of throughput, 1300~1500W of power, 500~800r/min of pump speed, 15~30ml/ of oxygen
Min, cryogenic temperature -10~-20 DEG C, quarter bend position -1mm；
Preferably, the condition of emission spectrum is：Plasma flow amount 18L/min, secondary air amount 1.0L/min, atomization
Device throughput 0.3L/min, power 1400W, pump speed 600r/min, oxygen 20ml/min, -15 DEG C of cryogenic temperature, quarter bend position -
1mm。
And by carrying out the detection of impurity levels first for unstrpped gas, also can for raw material composition situation more
Add understanding, be also beneficial to subsequently during the reaction, silicone content in product is effectively pre-adjusted and controlled.
Embodiment 1
As follows, the sample to be tested of unstripped gas is obtained：
1,25ml pressure resistance glass sample containers are placed in pipette, extract bright sulfur acid, 15% (about 4.5mL) of test tube is added, it is close
Envelope.
2, the sample in high-pressure glass sampling bottle is added to double-ended needle in high-pressure glass sampler, test tube is added
65% (about 19.5mL)；
3, high-pressure glass sampler is rocked into about 1min, and placed 30 minutes, observe its response situation.
4, it deflated, bled off pressure to high-pressure glass sampler with syringe needle.
5, steel cylinder without gas, without pressure after, open sealing cover, by gained dilute 40 times (weighing 0.5g adds white oil to 20g), as
Sample to be tested.
Experimental example 1
Step as follows carries out silicone content detection to the sample to be tested prepared by embodiment 1：
1, standard specimen is prepared, after isooctene standard items are diluted to 40 times of quality with white oil, as standard specimen；
2, argon gas air source is opened, checks that argon gas gross pressure should be in 6MPa or more, pressure is 0.8MPa after decompression；
3, refrigeration electromechanical source is opened.Check refrigeration machine working condition.(cryogenic temperature is 22 DEG C)；
4, air compressor power supply is opened.Check air pressure (0.8MPa)；
5, sample introduction refrigerator (- 15 DEG C) is opened；Meanwhile ICP extract systems should start to work；
6, work station is opened, sample analysis method (external standard addition method) is established；
7, ICP testing conditions are as follows：
Plasma flow amount 18L/min, secondary air amount 1.0L/min, atomizer throughput 0.3L/min, power
1400W, pump speed 600r/min, oxygen 20ml/min, -15 DEG C of cryogenic temperature, quarter bend position -1mm；
8, check whether each air source is normal, and whether temperature is normal；
9, ICP power supplys are opened, put torch after ten minutes；
10, oxygen valve is opened after 2 minutes, it is about 20ml/ minutes to adjust flow；
11, pump line is installed, and checks whether normal, progress next step operation when normal；
12, analysis margin, blank intensity value to stabilization (about 30~40 minutes)；
13, standard curve is done with standard addition method, related coefficient is at least three 9；Meanwhile when sample introduction, mixing standard specimen is answered；
14, sample is analyzed；It surveys analysis sample time to complete at 30 minutes, time-out should do standard curve again；
15, redeterminate sample when addition method standard specimen, as a result in error range when, illustrate that this surveys all samples
The result of product is effective, otherwise reforms standard curve, makees sample again.
Experimental example 2
According to the method for experimental example 1, silicone content detection is carried out to four unstripped gas of carbon after the ether of different batches；Meanwhile it detecting
Silicone content in the isooctane produced by corresponding batch unstripped gas, the results are shown in table below：
By upper table data it is found that detection method can accurately examine the silicone content in four raw material of carbon after ether
It surveys, and this testing result also can accurately reflect the level of the silicone content in finished product isooctane.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from the present invention's
Many other change and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (9)
1. a kind of detection method for producing silicone content in four unstripped gas of carbon after the ether of isooctane, which is characterized in that the inspection
Survey method includes the following steps：
(a) bright sulfur acid is added to the container, is sealed；
(b) into container be added ether after four unstripped gas sample of carbon；
(c) container is rocked so that four unstripped gas sample of carbon reacts in a reservoir after ether；
(d) after reaction, it deflated, bled off pressure to container；
(e) reaction product layer is taken, is diluted；Then, using ICP external standard methods, the silicone content in product is detected.
2. detection method according to claim 1, which is characterized in that the addition of bright sulfur acid be container volume 12~
18%；
Preferably, the addition of bright sulfur acid is the 15~17% of container volume.
3. detection method according to claim 1, which is characterized in that in the detection method, after still further comprising ether
The step of four unstripped gas sample of carbon.
4. detection method according to claim 3, which is characterized in that four unstripped gas sample of carbon includes following step after ether
Suddenly：
Sampler is connected to four unstripped gas sample storage tank of carbon after ether, after opening storage tank valve, discharge gas is to there is liquid, so
After collect liquid, four unstripped gas sample of carbon as after ether.
5. detection method according to claim 1, which is characterized in that the addition of four unstripped gas sample of carbon is container after ether
The 60~70% of volume；
Preferably, the addition of four unstripped gas sample of carbon is the 60~65% of container volume after ether.
6. detection method according to claim 1, which is characterized in that in step (c), the time for rocking container is 1
~5min；
Preferably, in step (c), further include after rocking container, the step of placement that container is static.
7. detection method according to claim 1, which is characterized in that be diluted to product dilution extremely described in step (e)
30~50 times；
Preferably, it states and is diluted to product dilution to 40~50 times.
8. detection method according to claim 1, which is characterized in that be diluted to product with white oil in step (e).
9. detection method according to claim 1, which is characterized in that the spectral conditions in step (e) are：
Plasma flow 15~20L/min of amount, 0.5~1.5L/min of secondary air amount, 0.1~0.5L/ of atomizer throughput
Min, 1300~1500W of power, 500~800r/min of pump speed, 15~30ml/min of oxygen, cryogenic temperature -10~-20 DEG C, square
1~-1mm of pipe position.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810418308.6A CN108459015B (en) | 2018-05-04 | 2018-05-04 | Method for detecting silicon content in etherified four-carbon raw material gas for producing isooctane |
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|---|---|---|---|
| CN201810418308.6A CN108459015B (en) | 2018-05-04 | 2018-05-04 | Method for detecting silicon content in etherified four-carbon raw material gas for producing isooctane |
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Inventor after: Lu Hongyong Inventor after: Bai Lu Inventor before: Lu Hongyong Inventor before: Bai Lu Inventor before: Wang Suqin Inventor before: Cao Yuanyuan |