CN108459015B - Method for detecting silicon content in etherified four-carbon raw material gas for producing isooctane - Google Patents
Method for detecting silicon content in etherified four-carbon raw material gas for producing isooctane Download PDFInfo
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- CN108459015B CN108459015B CN201810418308.6A CN201810418308A CN108459015B CN 108459015 B CN108459015 B CN 108459015B CN 201810418308 A CN201810418308 A CN 201810418308A CN 108459015 B CN108459015 B CN 108459015B
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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 invention provides a method for detecting the silicon content in a carbon four-raw material gas after production of ether of isooctane. The detection method comprises the following steps: (a) adding pure sulfuric acid into a container, and sealing; (b) adding a sample of the etherified C-C feed gas to the vessel; (c) shaking the container to enable the etherified carbon four-raw material gas sample to react in the container; (d) after the reaction is finished, the container is deflated and decompressed; (e) taking the upper reaction product and diluting the upper reaction product; and then, detecting the silicon content in the product by adopting an ICP external standard method. The detection method can indirectly detect the silicon content in the feed gas by a spectrum method, greatly improves the expectation of the silicon content in the final isooctane product, and improves the production efficiency; meanwhile, the detection method provided by the invention is simple and convenient in steps, high in detection efficiency, high in detection result accuracy and good in repeatability, and can accurately reflect the silicon content level in the feed gas.
Description
Technical Field
The invention relates to the field of chemical spectrum detection, in particular to a method for detecting silicon content in ether-produced carbon four-raw material gas for producing isooctane.
Background
At present, an alkylation device is a main process for producing isooctane, silicon content in carbon four after ether used in alkylation production is completely transferred to finished products of isooctane in the production process, the index of silicon content of isooctane is a very key index, once the index of silicon content in raw material gas exceeds the standard, the silicon content in the finished products exceeds the standard, the finished products with the silicon content exceeding the standard are difficult to be subjected to next treatment so as to enable the silicon content to reach the standard, certain difficulty is brought to production, and great waste is caused to enterprises. Further, in the conventional methods, there has been no study concerning the detection of silicon in the raw material.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a method for detecting the silicon content in the carbon four raw material gas after the production of the ether of isooctane, which has the advantages of simplicity, convenience, high efficiency, accurate detection result and the like.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
a detection method for silicon content in a carbon four-raw material gas after ether production for isooctane comprises the following steps:
(a) adding pure sulfuric acid into a container, and sealing;
(b) adding a sample of the etherified C-C feed gas to the vessel;
(c) shaking the container to enable the etherified C-C raw material gas sample to react;
(d) after the reaction is finished, the container is deflated and decompressed;
(e) taking the upper reaction product and diluting the upper reaction product; and then, detecting the silicon content in the product by adopting an ICP external standard method.
Preferably, in the detection method, the addition amount of the pure sulfuric acid is 12-18% of the volume of the container;
more preferably, the addition amount of the pure sulfuric acid is 15-17% of the volume of the container.
Preferably, the detection method further comprises a step of sampling a sample of the post-etherification carbon four raw material gas.
Preferably, in the detection method of the present invention, sampling a sample of the post-etherification carbon four-raw material gas includes the following steps:
and communicating the sampler with the ether-containing C-C raw material gas sample storage tank, opening a valve of the storage tank, discharging gas until liquid appears, and collecting the liquid, namely the ether-containing C-C raw material gas sample.
Preferably, in the detection method, the adding amount of the etherified carbon four raw material gas sample is 60-70% of the volume of the container;
more preferably, the adding amount of the etherified carbon four raw material gas sample is 60-65% of the volume of the container.
Preferably, in the step (c) of the detection method of the present invention, the time for shaking the container is 1-5 min;
more preferably, the step (c) further comprises the step of placing the container still after shaking the container.
Preferably, in the detection method of the invention, the dilution in the step (e) is to dilute the product to 30-50 times;
more preferably, the dilution is to dilute the product to 40-50 times.
Preferably, in step (e) of the detection method of the present invention, the product is diluted with white oil.
Preferably, in the step (e) of the detection method of the present invention, the spectral conditions are:
the plasma gas flow is 15-20L/min, the auxiliary gas flow is 0.5-1.5L/min, the atomizer gas flow is 0.1-0.5L/min, the power is 1300-1500W, the pump speed is 500-800 r/min, the oxygen is 15-30 ml/min, the refrigeration temperature is-10 to-20 ℃, and the rectangular tube position is 1 to-1 mm.
Compared with the prior art, the invention has the beneficial effects that:
the detection method can indirectly detect the silicon content in the feed gas by a spectrum method, greatly improves the expectation of the silicon content in the final isooctane product, and improves the production efficiency;
meanwhile, the detection method provided by the invention is simple and convenient in steps, high in detection efficiency, high in detection result accuracy and good in repeatability, and can accurately reflect the silicon content level in the feed gas.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is a schematic structural diagram of a post-etherification carbon four-raw material sampling device according to an embodiment of the present invention;
FIG. 2 is a schematic structural view of a device for performing the air bleeding and pressure releasing steps provided in the embodiment of the present invention;
fig. 3 is a schematic structural diagram of a product sampling step device provided in the embodiment of the present invention.
In the figure 1, a 1-ether post-carbon four-raw material pipeline, a 2-ether post-carbon four-raw material pipeline sampling pipeline, a 3-sampling valve, a 4-double-ended needle and a 5-pressure-resistant glass sampler are arranged;
in FIG. 2, 1-syringe needle, 2-sealed container;
in FIG. 3, 1-vessel, 2-pipette, 3-product, 4-mix material.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In view of the fact that the existing method does not have relevant research on detection of the silicon content in the isooctane raw material gas, the invention particularly provides a method for detecting the silicon content in the isooctane raw material gas, and accurate reflection of the silicon content level in the raw material gas is realized through convenient and rapid detection steps, so that the production efficiency is improved.
The detection method provided by the invention can refer to the following steps:
(a) adding pure sulfuric acid into a container, and sealing;
in this step, the addition amount of the pure sulfuric acid is preferably controlled to be 12-18% of the volume of the container (calibration volume), for example, but not limited to 13, 14, 15, 16, or 17%; preferably, the adding amount of the pure sulfuric acid is 15-17% of the volume of the container;
the pure sulfuric acid is mainly used for playing a catalytic role, the olefin in the etherified C4 is polymerized under the catalytic action of the sulfuric acid to obtain isooctane, and then the silicon content in the product isooctane is detected by using a spectral detection method, so that the silicon content level in the etherified C4 raw material is indirectly reflected.
Since the etherified carbon four raw material exists in the form of a gas (liquefied gas), it cannot be detected for impurity components (e.g., silicon, etc.) by spectroscopy; after the catalyst is polymerized, impurity compounds such as silicon and the like in the reacted etherified carbon four raw material still can be contained in the product (the silicon impurities in the very small amount of unreacted etherified carbon four raw material cannot react with pure sulfuric acid, so that the silicon impurities are still wrapped in the etherified carbon four gas raw material, and the accuracy of the detection result cannot be influenced). Therefore, by detecting the silicon content in this portion of the product, the content level of impurities such as silicon in the raw material C4 can be obtained.
Meanwhile, in the step, the container is a pressure-resistant container; since the etherified tetracarbon compound is further added to the vessel in the form of liquefied gas, the reaction process is an exothermic reaction, resulting in an increase in the temperature of the vessel and an increase in the internal pressure. Therefore, the container used in the present invention is preferably a heat-resistant pressure-resistant container;
further, in order to facilitate observation of the reaction progress, the vessel used in the present invention is preferably a pressure-resistant glass sampler.
(b) Adding a sample of the etherified C-C feed gas to the vessel;
in this step, before the raw material gas sample is added, a sampling step is further included, please refer to fig. 1, which includes:
one end of a double-ended needle 4 is connected with a sampling pipeline 2 of the etherified carbon four-material line;
then, opening a sampling valve 3, discharging the etherified carbon four-raw material gas from the etherified carbon four-raw material pipeline 1, and continuously discharging the gas until liquid (namely etherified carbon four-raw material liquefied gas) appears;
then a pressure-resistant glass sampler 5 connected with the other end of the double-ended needle 4 collects liquid, namely the etherified carbon four-raw material gas sample (namely, the raw material gas is liquefied gas, and the liquefied gas in a liquid state is used as the raw material, so that the raw material is convenient to transfer and measure, the polymerization reaction is effectively and massively carried out, and the accuracy of a detection result is ensured).
The collected feed gas is then fed into a sealed vessel containing pure sulfuric acid (preferably, the collected feed gas may be introduced into the reaction vessel using a double-ended needle).
In this step, the amount of the etherified four-carbon raw material gas sample added is 60-70% of the volume of the container, for example, but not limited to, 61, 62, 63, 64, 65, 66, 67, 68, 69% or the like; preferably, the adding amount of the etherified carbon four raw material gas sample is 60-65% of the volume of the container;
further, due to the exothermic reaction and the endothermic gasification volume expansion of the liquefied gas C4, the total amount of pure sulfuric acid and raw gas should be controlled to be less than 85% of the container volume in order to ensure the safety during the detection process.
(c) Shaking the container to enable the etherified carbon four-raw material gas sample to react in the container;
after the addition of pure sulfuric acid and the etherified carbon four raw material gas is finished, shaking the container to enable the pure sulfuric acid and the etherified carbon four raw material gas to be fully contacted, and generating isooctane from the etherified carbon four raw material gas under the catalysis of concentrated sulfuric acid;
preferably, the shaking time of the container is 1-5 min, for example, but not limited to, 2, 3, or 4 min;
further, after the raw material is fully contacted with the sulfuric acid by shaking, the step further comprises a step of standing after shaking, so that the etherified C-C raw material gas can be fully subjected to polymerization reaction;
the time for standing is preferably controlled to be 15-45 min, for example, but not limited to, 20, 25, 30min and the like;
in the standing process, the reaction condition in the container is observed, so that the danger is avoided.
(d) After the reaction is finished, the container is deflated and decompressed;
referring to fig. 2, after the reaction is completed, the sealed container 2 is released from the gas and pressure by the syringe needle 1, and the gasified ether-carbon four-source liquefied gas which is not subjected to the polymerization reaction is discharged.
(e) Taking a reaction product, and diluting the reaction product; and then, detecting the silicon content in the product by adopting an ICP external standard method.
Opening the sealing cover after the container is free of air and pressure; then, taking out the product from the upper part, and diluting;
referring to fig. 3, the product sampling steps are as follows: taking out the upper layer of the product 3 of the container 1 by using a pipette 2, and taking out the lower layer of the mixed material 4;
the mixed feed 4 is mainly pure sulfuric acid as catalyst, and small amounts of other products.
Preferably, the product is diluted 30 to 50 times with white oil, for example, but not limited to, the product is diluted 35, 40, or 45 times with white oil.
Then, the diluted product was subjected to ICP (emission spectroscopy) and the silicon content was measured by the external standard method.
Furthermore, the standard sample is also diluted with white oil before the spectroscopic detection, and the dilution ratio is the same as that of the product to be detected.
Meanwhile, the emission spectrum conditions are: the plasma gas flow is 15-20L/min, the auxiliary gas flow is 0.5-1.5L/min, the atomizer gas flow is 0.1-0.5L/min, the power is 1300-1500W, the pump speed is 500-800 r/min, the oxygen is 15-30 ml/min, the refrigeration temperature is-10 to-20 ℃, and the rectangular tube position is-1 mm;
preferably, the emission spectrum is conditioned by: the plasma gas flow is 18L/min, the auxiliary gas flow is 1.0L/min, the atomizer gas flow is 0.3L/min, the power is 1400W, the pump speed is 600r/min, the oxygen is 20ml/min, the refrigeration temperature is-15 ℃, and the position of a rectangular tube is-1 mm.
And through the detection of the content of the silicon impurities in the raw material gas, the composition condition of the raw material can be known better, and the effective pre-adjustment and control of the silicon content in the product in the subsequent reaction process are facilitated.
Example 1
Obtaining a sample to be tested of the raw material gas according to the following method:
1. the pure sulfuric acid was pipetted into a 25mL pressure-resistant glass sampler, 15% of the tube (about 4.5mL) was added, and the tube was sealed.
2. The sample in the high pressure glass sampling bottle was added to the high pressure glass sampler using a double ended needle, adding 65% of the test tube (about 19.5 mL);
3. the high pressure glass sampler was shaken for about 1min and left to stand for 30 minutes, and the reaction was observed.
4. And (4) deflating and decompressing the high-pressure glass sampler by using the needle.
5. After the steel cylinder is free of air and pressure, the sealing cover is opened, and the obtained mixture is diluted by 40 times (0.5 g of white oil is added to 20g), namely the sample to be detected is obtained.
Experimental example 1
The silicon content of the sample to be tested prepared in example 1 was tested according to the following method steps:
1. preparing a standard sample, and diluting an isooctene standard substance to 40 times of the mass by using white oil to obtain the standard sample;
2. opening an argon source, checking that the total pressure of argon is more than 6MPa, and reducing the pressure to 0.8 MPa;
3. and turning on the power supply of the refrigerator. Checking the working state of the refrigerator. (refrigeration temperature 22 ℃);
4. and turning on the power supply of the air compressor. Checking the air pressure (0.8 MPa);
5. opening the sample refrigerator (-15 ℃); meanwhile, the ICP air exhaust system should start to work;
6. opening a work station, and establishing a sample analysis method (external standard addition method);
7. the ICP detection conditions were as follows:
the plasma gas flow is 18L/min, the auxiliary gas flow is 1.0L/min, the atomizer gas flow is 0.3L/min, the power is 1400W, the pump speed is 600r/min, the oxygen is 20ml/min, the refrigeration temperature is-15 ℃, and the rectangular tube position is-1 mm;
8. checking whether each gas source is normal and whether the temperature is normal;
9. turning on an ICP power supply, and igniting the torch after 10 minutes;
10. opening an oxygen valve after 2 minutes, and regulating the flow rate to be about 20 ml/minute;
11. installing a pump pipe, checking whether the pump pipe is normal or not, and performing the next operation when the pump pipe is normal;
12. analyzing the blank, and enabling the blank intensity value to be stable (about 30-40 minutes);
13. a standard addition method is used for making a standard curve, and the minimum correlation coefficient is three 9; meanwhile, when sampling, the standard sample is uniformly mixed;
14. analyzing the sample; the time for measuring and analyzing the sample is finished within 30 minutes, and a standard curve is made again after the time is out;
15. and re-measuring the samples used in the adding method standard sample, wherein when the result is within the error range, the result of all the samples measured at this time is effective, otherwise, re-preparing the standard curve and re-preparing the sample.
Experimental example 2
According to the method of experimental example 1, silicon content detection is carried out on different batches of etherified C-C raw material gases; meanwhile, the silicon content in isooctane produced from the corresponding batch of raw material gas was measured, and the results are shown in the following table:
the data in the table show that the detection method can accurately detect the silicon content in the etherified carbon four raw material, and the detection result can also accurately reflect the silicon content level in finished isooctane.
While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (4)
1. A detection method for silicon content in a carbon four-raw material gas after ether production for isooctane is characterized by comprising the following steps:
(a) adding pure sulfuric acid into a container, and sealing;
(b) adding a sample of the etherified C-C feed gas to the vessel;
(c) shaking the container to enable the etherified carbon four-raw material gas sample to react in the container;
(d) after the reaction is finished, the container is deflated and decompressed;
(e) taking the upper reaction product and diluting the upper reaction product; then, detecting the silicon content in the product by adopting an ICP external standard method;
the adding amount of the pure sulfuric acid is 12-18% of the volume of the container;
the detection method also comprises the step of sampling a four-carbon raw material gas sample after the etherification;
sampling of the etherified carbon four-raw material gas comprises the following steps:
communicating the sampler with a storage tank of the etherified C-C raw material gas sample, opening a valve of the storage tank, discharging the gas until liquid appears, and collecting the liquid, namely the etherified C-C raw material gas sample;
the adding amount of the etherified C-C raw material gas sample is 60-70% of the volume of the container;
in the step (c), the container is shaken for 1-5 min;
in the step (c), the method further comprises the step of placing the container in a static state after shaking the container;
diluting the product to 30-50 times in the step (e);
in the step (e), the product is diluted by white oil;
the spectral conditions in step (e) are:
the plasma gas flow is 15-20L/min, the auxiliary gas flow is 0.5-1.5L/min, the atomizer gas flow is 0.1-0.5L/min, the power is 1300-1500W, the pump speed is 500-800 r/min, the oxygen is 15-30 ml/min, the refrigeration temperature is-10 to-20 ℃, and the rectangular tube position is 1 to-1 mm.
2. The method for detecting the content of silicon in the etherified carbon four raw material gas for producing isooctane according to claim 1, wherein the amount of pure sulfuric acid added is 15-17% of the volume of the container.
3. The method for detecting the content of silicon in the etherified carbon four-source gas used for producing isooctane according to claim 1, wherein the amount of the added etherified carbon four-source gas sample is 60-65% of the volume of the container.
4. The method for detecting the content of silicon in the etherified four-carbon raw material gas for producing isooctane according to claim 1, wherein the dilution is to dilute the product by 40-50 times.
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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 |