CN111983134B - Method for measuring contents of hydrogen sulfide and hydrogen polysulfide in liquid sulfur - Google Patents
Method for measuring contents of hydrogen sulfide and hydrogen polysulfide in liquid sulfur Download PDFInfo
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Abstract
The invention discloses a method for measuring the content of hydrogen sulfide and hydrogen polysulfide in liquid sulfur, and belongs to the field of chemical component detection. The method comprises the following steps: taking a first liquid sulfur sample from the liquid sulfur mother liquor; mixing a first liquid sulfur sample with a catalyst and heating to a preset temperature to obtain a target solution; inserting a first protective gas exhaust pipe into the target solution to enable the first protective gas to purge the target solution; carrying out iodometry measurement on the purged gas to obtain the total hydrogen sulfide content in the first liquid sulfur sample; and determining the content of hydrogen sulfide and hydrogen polysulfide in the liquid sulfur mother liquor according to the total content of hydrogen sulfide. The method is convenient to operate, does not need to use combustible and toxic reagents, can avoid environmental pollution, can prevent the body health of operators from being damaged quickly, is simple to operate, and can effectively and accurately measure the hydrogen sulfide content and the hydrogen polysulfide content in the liquid sulfur mother liquor.
Description
Technical Field
The invention relates to the field of chemical component detection, in particular to a method for determining the content of hydrogen sulfide and hydrogen polysulfide in liquid sulfur.
Background
In oil refining and natural gas purification processes, liquid sulfur is typically recovered. Wherein, the liquid sulfur has residual hydrogen sulfide, the residual hydrogen sulfide reacts with the sulfur at high temperature to form hydrogen polysulfide, and the hydrogen polysulfide is decomposed into hydrogen sulfide and sulfur at room temperature. Once discharged into the atmosphere, this hydrogen sulfide not only pollutes the environment, but also causes physical health damage to the workers involved. Therefore, it is necessary to detect the total hydrogen sulfide (including hydrogen sulfide and hydrogen polysulfide) content in the liquid sulfur to ensure that the total hydrogen sulfide content in the liquid sulfur is lower than the national standard.
Currently, potentiometry is commonly used to detect the total hydrogen sulfide content in liquid sulfur. However, this method requires the use of flammable and toxic chemicals, which not only pollutes the environment, but also causes the physical health of the operator to be impaired.
Disclosure of Invention
The embodiment of the invention provides a method for measuring the content of hydrogen sulfide and hydrogen polysulfide in liquid sulfur, which can solve the technical problem. The technical scheme is as follows:
a method for determining the content of hydrogen sulfide and hydrogen polysulfide in liquid sulfur, comprising:
taking a first liquid sulfur sample from the liquid sulfur mother liquor;
uniformly mixing the first liquid sulfur sample with a catalyst and heating to a preset temperature to obtain a target solution;
inserting a first protective gas exhaust tube into the target solution to allow a first protective gas to purge the target solution, wherein the first protective gas exhaust tube is inserted at least two-thirds of the depth of the target solution;
carrying out iodometry measurement on the purged gas to obtain the total hydrogen sulfide content in the first liquid sulfur sample;
and determining the content of hydrogen sulfide and hydrogen polysulfide in the liquid sulfur mother liquor according to the total content of hydrogen sulfide.
In one possible design, the preset temperature is the temperature of the liquid sulphur mother liquor, and the difference between the preset temperature and the melting point of the catalyst is at most 30 ℃.
In one possible design, the catalyst is picric acid.
In one possible design, the mass ratio of the catalyst to the first liquid sulfur sample is 1: (80-120).
In one possible design, the mass ratio of the catalyst to the first liquid sulfur sample is 1: 100.
in one possible design, the first protective gas is nitrogen.
In one possible design, the purge time of the first protective gas is 110min to 130 min.
In one possible design, the determining the hydrogen sulfide and hydrogen polysulfide content in the liquid sulfur mother liquor from the total hydrogen sulfide content comprises:
determining a chemical equilibrium constant corresponding to the liquid sulfur mother liquor according to the temperature of the liquid sulfur mother liquor;
and calculating to obtain the contents of hydrogen sulfide and hydrogen polysulfide in the liquid sulfur mother liquor according to the chemical equilibrium constant and the total hydrogen sulfide content.
In one possible design, the determining the hydrogen sulfide and hydrogen polysulfide content in the liquid sulfur mother liquor from the total hydrogen sulfide content comprises:
removing a second liquid sulfur sample from the liquid sulfur mother liquor;
purging the second liquid sulfur sample by using a second protective gas, and carrying out iodometry measurement on the purged gas to obtain the hydrogen sulfide content in the second liquid sulfur sample;
and subtracting the hydrogen sulfide content from the total hydrogen sulfide content to determine the hydrogen polysulfide content in the liquid sulfur mother liquor.
In one possible design, the purge time of the second shielding gas is 230min to 250 min.
The technical scheme provided by the embodiment of the invention has the beneficial effects that at least:
according to the determination method provided by the embodiment of the invention, the catalyst is added into the first liquid sulfur sample and is uniformly mixed, so that the equilibrium reaction in the first liquid sulfur sample is carried out under the catalytic action of the catalyst
The sulfur dioxide is broken and moves towards the direction of generating hydrogen sulfide, so that the hydrogen sulfide and the hydrogen polysulfide in the first liquid sulfur sample continuously purge through the first protective gas and escape from the target solution, thereby obtaining the total hydrogen sulfide content in the first liquid sulfur sample, and further, the content of the hydrogen sulfide and the hydrogen polysulfide in the first liquid sulfur sample can be traced according to the total hydrogen sulfide content in the first liquid sulfur sample, so that the content of the hydrogen sulfide and the hydrogen polysulfide in the liquid sulfur mother liquor can be determined. Therefore, the determination method provided by the embodiment of the invention is convenient to operate, does not need combustible and toxic reagents, can avoid environmental pollution, can prevent the physical health of operators from being damaged, is simple to operate, and can effectively and accurately determine the content of hydrogen sulfide and the content of hydrogen polysulfide in the liquid sulfur mother liquor.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a flow chart of a method for determining the content of hydrogen sulfide and hydrogen polysulfide in liquid sulfur according to an embodiment of the present invention;
FIG. 2 is a flow chart of a method for determining the content of hydrogen sulfide and hydrogen polysulfide in another type of liquid sulfur according to an embodiment of the present invention;
FIG. 3 is a flow chart of a method for determining the content of hydrogen sulfide and hydrogen polysulfide in another type of liquid sulfur according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
It should be noted that the total hydrogen sulfide content in the examples of the present invention refers to the sum of the contents of hydrogen sulfide and hydrogen polysulfide.
The embodiment of the invention provides a method for measuring the content of hydrogen sulfide and hydrogen polysulfide in liquid sulfur, which comprises the following steps of:
step S1, a first liquid sulfur sample is taken out of the liquid sulfur mother liquor.
And step S2, mixing the first liquid sulfur sample with a catalyst and heating to a preset temperature to obtain a target solution.
And step S3, inserting a first protective gas exhaust pipe into the target solution to enable the first protective gas to purge the target solution, wherein the first protective gas exhaust pipe is inserted at least to two thirds of the depth of the target solution.
And step S4, carrying out iodometry measurement on the purged gas to obtain the total hydrogen sulfide content in the first liquid sulfur sample.
And step S5, determining the content of hydrogen sulfide and hydrogen polysulfide in the liquid sulfur mother liquor according to the content of the total hydrogen sulfide.
According to the determination method provided by the embodiment of the invention, the catalyst is added into the first liquid sulfur sample and is uniformly mixed, so that the equilibrium reaction in the first liquid sulfur sample is carried out under the catalytic action of the catalyst
The sulfur dioxide is broken and moves towards the direction of generating hydrogen sulfide, so that the hydrogen sulfide and the hydrogen polysulfide in the first liquid sulfur sample continuously purge through the first protective gas and escape from the target solution, thereby obtaining the total hydrogen sulfide content in the first liquid sulfur sample, and further, the content of the hydrogen sulfide and the hydrogen polysulfide in the first liquid sulfur sample can be traced according to the total hydrogen sulfide content in the first liquid sulfur sample, so that the content of the hydrogen sulfide and the hydrogen polysulfide in the liquid sulfur mother liquor can be determined. Therefore, the determination method provided by the embodiment of the invention is convenient to operate, does not need combustible and toxic reagents, can avoid environmental pollution, can prevent the physical health of operators from being damaged, is simple to operate, and can effectively and accurately determine the content of hydrogen sulfide and the content of hydrogen polysulfide in the liquid sulfur mother liquor.
The following describes the steps of the assay method provided in the examples of the present invention:
in step S1, the liquid sulfur mother liquor refers to liquid sulfur recovered in the petroleum refining and natural gas purification processes.
For step S2, it can specifically be: and adding a first liquid sulfur sample into a container filled with the catalyst, and heating to a preset temperature to uniformly mix the catalyst and the first liquid sulfur sample to obtain a target solution.
According to the embodiment of the invention, the catalyst is placed at the bottom of the container, and the first liquid sulfur sample is added at the upper part of the catalyst, so that the catalyst can be gradually melted when the bottom of the container is heated, and the first liquid sulfur sample can be fully melted into the catalyst, so that the uniformly mixed target solution is obtained, and the catalytic effect and the utilization rate of the catalyst are improved.
Wherein, due to equilibrium reaction in the first liquid sulfur
Is related to the temperature of the liquid sulphur precursor, ifTo determine the hydrogen sulfide and hydrogen polysulfide content of the liquid sulfur mother liquor, the temperature of the first liquid sulfur sample is to be consistent with the temperature of the liquid sulfur mother liquor to improve the accuracy of the determination. In addition, when the melting point of the catalyst is less than the temperature of the liquid sulfur mother liquor and the difference between the two temperature differences is not large, the catalyst can be completely melted into liquid when the bottom of the container is heated to the temperature of the liquid sulfur mother liquor in the container, and can be uniformly mixed with the first liquid sulfur sample, so that the catalytic effect of the catalyst is improved. Then, the preset temperature in this step may be the temperature of the liquid sulfur mother liquor, and the difference between the preset temperature and the melting point of the catalyst is at most 30 ℃, and may be, for example, 5 ℃, 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃, and the like.
Wherein, when the total hydrogen sulfide concentration of the first liquid sulfur sample is lower than 100ug/g, the heating time may be 15min to 25min, for example, 15min, 17min, 19min, 21min, 23min, 25min, etc.; when the total hydrogen sulfide concentration of the first liquid sulfur sample is greater than 100ug/g, the heating time may be 5min to 15min, for example, 5min, 7min, 9min, 11min, 13min, 15min, etc. The same liquid sulfur sample is divided into a plurality of parts from the beginning of sampling to the time when the sample is placed in a sample window, different times are respectively adopted for starting tests, the change of the infrared spectrum (absorbance) of each liquid sulfur sample along with the time is measured, a result is obtained, and according to the test result, when the total hydrogen sulfide concentration in the liquid sulfur sample is less than 5ug/g, the total hydrogen sulfide content is not changed within 120min in the measuring process; when the concentration of the total hydrogen sulfide in the liquid sulfur sample is 5 ug/g-10 ug/g, the analysis result of the total hydrogen sulfide content is not changed within 40 min; when the concentration of the total hydrogen sulfide in the liquid sulfur sample is 10 ug/g-25 ug/g, the change of the total hydrogen sulfide content is smaller within 40 min; when the concentration of the total hydrogen sulfide in the liquid sulfur sample is 25 ug/g-50 ug/g, the analysis result of the total hydrogen sulfide content is unchanged within 30 min; when the concentration of the total hydrogen sulfide in the liquid sulfur sample is 50 ug/g-100 ug/g, the total hydrogen sulfide content is not lost within 40 minutes; when the concentration of the total hydrogen sulfide in the liquid sulfur sample is between 100ug/g and 200ug/g, the total hydrogen sulfide content is not lost within 15 min; when the concentration of the total hydrogen sulfide in the liquid sulfur sample is 200 ug/g-300 ug/g, the total hydrogen sulfide content is not lost within 40 min.
In addition, in the embodiment of the invention, the catalyst can be picric acid. The melting point of the picric acid is 121.8 ℃, which is equivalent to the temperature of the liquid sulfur mother liquor (mostly about 145 ℃), so that the picric acid can be completely melted into liquid when the bottom of the container is heated to the temperature of 145 ℃ inside the container, and can be uniformly mixed with the first liquid sulfur sample, and the catalytic effect of the catalyst can be further improved.
Further, based on the catalyst with the above components, in the embodiment of the present invention, the mass ratio of the catalyst to the first liquid sulfur sample is 1: (80-120), for example, the ratio of 1: 80. 1: 90. 1: 100. 1: 110. 1: 120, etc. Through such setting, can make the catalyst reach the catalytic effect to first liquid sulphur sample effectively, can improve the survey precision of total hydrogen sulfide content in the first liquid sulphur sample.
Further, the mass ratio of the catalyst to the first liquid sulfur sample is 1: 100. through such setting, can make the catalyst reach the catalytic effect to first liquid sulphur sample effectively, can improve the survey precision of total hydrogen sulfide content in the first liquid sulphur sample.
In step S3, a first protective gas exhaust pipe communicating with the first protective gas tank is inserted into the target solution, and then the target solution is purged by introducing gas into the target solution. Wherein the first protective gas exhaust pipe is inserted at least two thirds of the depth of the target solution.
By setting the insertion depth of the first protective gas exhaust pipe in this way, the first protective gas can smoothly enter the target solution, and the gas in the target solution can be completely purged out, so that the measurement accuracy of the content of hydrogen sulfide and hydrogen polysulfide in the liquid sulfur mother liquor can be improved.
In addition, the first protective gas in this step may be nitrogen, hydrogen, or an inert gas (e.g., helium, argon), or the like. In view of the characteristics of convenient acquisition and low price of nitrogen, the embodiment of the invention is preferably adopted.
Considering that, after the first liquid sulfur sample is taken out from the liquid sulfur mother liquor, due to external factors, hydrogen sulfide in the first liquid sulfur sample can escape, so that the measurement accuracy of the contents of hydrogen sulfide and hydrogen polysulfide in the liquid sulfur mother liquor is not high, and therefore, the time for purging the first protective gas cannot exceed a certain time, in the embodiment of the present invention, the purging time of the first protective gas is 110min to 130min, for example, may be set to 110min, 115min, 120min, 125min, 130min, and the like.
Furthermore, the purging time of the first protective gas can be 120min, so that all hydrogen sulfide and hydrogen polysulfide in the first liquid sulfur sample can be completely blown out, the time is saved, and the method is simple and easy to implement.
In step S4, iodometry measurement is performed on the purged gas to obtain the total hydrogen sulfide content in the first liquid sulfur sample.
The iodometry is a conventional iodometry, and may specifically be: the mass of hydrogen sulfide and hydrogen polysulfide purged off can be calculated by introducing the gas purged off with the first protective gas (e.g., nitrogen) into acetyl chloride to form a precipitate and back-titrating the precipitate with iodine.
For step S5, two methods can be used to determine the hydrogen sulfide and hydrogen polysulfide content in the liquid sulfur mother liquor. As shown in fig. 2, the first method includes:
and step S511, determining a chemical equilibrium constant corresponding to the liquid sulfur mother liquor according to the temperature of the liquid sulfur mother liquor.
Wherein, the chemical reaction formula of the liquid sulfur mother liquor is as follows:
the equilibrium constant K is equal to C H2S /C H2Sx . In the formula for calculating the equilibrium constant K, C is the total hydrogen sulfide content, C H2S Is hydrogen sulfide content, C H2Sx Is the hydrogen polysulfide content. The equilibrium constant K is related to the temperature of the liquid sulphur mother liquor, i.e. one temperature corresponds to one equilibrium constant K, for example at 145 ℃The equilibrium constant K is equal to 1.37.
Further, the equilibrium constant K can be determined by experiment, and taking the equilibrium constant K at 145 ℃ as an example, specifically, the content of hydrogen sulfide and hydrogen polysulfide in a plurality of liquid sulfur samples at a fixed temperature (145 ℃) is determined by an infrared spectrometer, the equilibrium constant at the temperature is calculated, and the value of the equilibrium constant K is 1.37 according to a weighted average method.
And S512, calculating to obtain the contents of hydrogen sulfide and hydrogen polysulfide in the liquid sulfur mother liquor according to the equilibrium constant and the total hydrogen sulfide content.
In particular, C may be expressed according to the formula H2S +C H2Sx And K ═ C H2S /C H2Sx And calculating to obtain the hydrogen sulfide content and the hydrogen polysulfide content in the liquid sulfur mother liquor.
As shown in fig. 3, the second method includes:
and step S521, taking out a second liquid sulfur sample from the liquid sulfur mother liquor.
The step may be specifically, a second liquid sulfur sample is taken out from the liquid sulfur mother liquor by using a container, wherein the quality of the second liquid sulfur sample may be the same as the quality of the first liquid sulfur sample.
And S522, purging the second liquid sulfur sample by using the second protective gas, and carrying out iodometry measurement on the purged gas to obtain the hydrogen sulfide content in the second liquid sulfur sample.
The step may specifically be inserting a second protective gas exhaust pipe communicated with a second protective gas tank into the second liquid sulfur sample, then ventilating the second liquid sulfur sample for purging, and performing iodometry measurement on the purged gas to obtain the hydrogen sulfide content in the second liquid sulfur sample.
The activation energy of hydrogen sulfide is lower than that of hydrogen polysulfide, and in the case where no catalyst is added to the second liquid sulfur sample, the gas purged with the second protective gas contains hydrogen sulfide gas and no hydrogen polysulfide gas. When the catalyst is added to the first liquid sulfur sample, the catalyst first reduces the activation energy of hydrogen sulfide, hydrogen sulfide material escapes first, and then hydrogen polysulfide gradually escapes under the action of the catalyst.
The second protective gas in this step may be nitrogen, hydrogen, or an inert gas (e.g., helium, argon), etc. In consideration of the characteristics of convenient acquisition and low price of nitrogen, the embodiment of the invention is preferably adopted.
Considering that the measurement accuracy of the hydrogen sulfide in the liquid sulfur mother liquor is not high due to the fact that the hydrogen sulfide in the second liquid sulfur sample escapes from the second liquid sulfur mother liquor due to external factors after the second liquid sulfur sample is taken out of the liquid sulfur mother liquor, the purging time of the second protective gas cannot exceed a certain time, in the embodiment of the invention, the purging time of the second protective gas is 230min to 250min, for example, 230min, 235min, 240min, 245min, 250min, and the like.
Furthermore, the purging time of the second protective gas is 240min, so that all hydrogen sulfide in the second liquid sulfur sample can be completely blown out, the time is saved, and the method is simple and feasible.
And step S523, subtracting the hydrogen sulfide content from the total hydrogen sulfide content to obtain the hydrogen polysulfide content in the liquid sulfur mother liquor.
The following describes a kind of measurement method provided in the embodiment of the present invention, taking an example as an example:
first, a first liquid sulfur sample and a second liquid sulfur sample of equal mass were taken out from a liquid sulfur mother liquor at a temperature of 145 ℃.
Secondly, mixing the components in a mass ratio of 1: 100 of picric acid was mixed uniformly with the first liquid sulfur sample and heated to 145 ℃ to obtain the target solution.
And secondly, purging the target solution for 2 hours by using nitrogen, and carrying out iodometry measurement on the purged gas to obtain the total hydrogen sulfide content in the first liquid sulfur sample. When the first liquid sulfur sample after nitrogen purging is taken to an infrared instrument for analysis, no peaks of hydrogen sulfide and hydrogen polysulfide exist in an infrared spectrogram, and an analysis result shows zero (shown in table 1), so that the hydrogen sulfide and the hydrogen polysulfide in the first liquid sulfur sample are fully purged by nitrogen purging for 2 hours under the action of the catalyst. Therefore, the total mass of hydrogen sulfide blown out by the catalyst chemical method is the total amount of hydrogen sulfide and hydrogen polysulfide in the liquid sulfur.
TABLE 1
And secondly, purging the second liquid sulfur sample for 4 hours by using nitrogen, and carrying out iodometry measurement on the purged gas to obtain the hydrogen sulfide content in the second liquid sulfur sample.
And finally, subtracting the hydrogen sulfide content from the total hydrogen sulfide content to obtain the hydrogen polysulfide content in the liquid sulfur mother liquor. The measurement results are shown in table 2.
TABLE 2
Therefore, compared with the purging determination method provided by the national standard and the purging determination method provided by the industrial standard, the determination method provided by the embodiment of the invention can ensure the accuracy of the determination result, is simple and convenient to operate, does not pollute the environment, and does not damage the body health of operators.
It should be noted that, at the present stage, the existing standard for determining the content of hydrogen sulfide in liquid sulfur in China is the national standard: industrial sulfur part 2: liquid products, and enterprise standards drafted by natural gas research institute of southwest oil and gas field division: chemical methods for determining residual hydrogen sulfide in sulfur produced by natural gas processing plants are shown in Table 3 below.
TABLE 3
All the above optional technical solutions may be combined arbitrarily to form the optional embodiments of the present disclosure, and are not described herein again.
The above description is only an illustrative embodiment of the present invention, and should not be taken as limiting the scope of the invention, and any modifications, equivalents, improvements and the like that are within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A method for measuring the content of hydrogen sulfide and hydrogen polysulfide in liquid sulfur is characterized by comprising the following steps:
taking a first liquid sulfur sample from the liquid sulfur mother liquor;
uniformly mixing the first liquid sulfur sample with a catalyst and heating to a preset temperature to obtain a target solution;
inserting a first protective gas exhaust tube into the target solution to allow a first protective gas to purge the target solution, wherein the first protective gas exhaust tube is inserted at least two-thirds of the depth of the target solution;
carrying out iodometry measurement on the purged gas to obtain the total hydrogen sulfide content in the first liquid sulfur sample;
determining the content of hydrogen sulfide and hydrogen polysulfide in the liquid sulfur mother liquor according to the total content of hydrogen sulfide;
the catalyst is picric acid, and the mass ratio of the catalyst to the first liquid sulfur sample is 1: 80-120 parts.
2. The assay according to claim 1, wherein the predetermined temperature is the temperature of the liquid sulphur mother liquor and the difference between the predetermined temperature and the melting point of the catalyst is at most 30 ℃.
3. The assay of claim 1, wherein the mass ratio of the catalyst to the first liquid sulfur sample is 1: 100.
4. the assay method of claim 1, wherein the first protective gas is nitrogen.
5. The method according to claim 4, wherein the purge time of the first protective gas is 110 to 130 min.
6. The method of claim 1, wherein said determining the hydrogen sulfide and hydrogen polysulfide content of said liquid sulfur mother liquor from said total hydrogen sulfide content comprises:
determining a chemical equilibrium constant corresponding to the liquid sulfur mother liquor according to the temperature of the liquid sulfur mother liquor;
and calculating to obtain the contents of hydrogen sulfide and hydrogen polysulfide in the liquid sulfur mother liquor according to the chemical equilibrium constant and the total hydrogen sulfide content.
7. The method of claim 1, wherein said determining the hydrogen sulfide and hydrogen polysulfide content of said liquid sulfur mother liquor from said total hydrogen sulfide content comprises:
removing a second liquid sulfur sample from the liquid sulfur mother liquor;
purging the second liquid sulfur sample by using a second protective gas, and carrying out iodometry measurement on the purged gas to obtain the hydrogen sulfide content in the second liquid sulfur sample;
and subtracting the hydrogen sulfide content from the total hydrogen sulfide content to determine the hydrogen polysulfide content in the liquid sulfur mother liquor.
8. The method according to claim 7, wherein the purge time of the second protective gas is 230 to 250 min.
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