CN113385155A - Reversible adsorbent for olefin content determination, and preparation method and application thereof - Google Patents

Reversible adsorbent for olefin content determination, and preparation method and application thereof Download PDF

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CN113385155A
CN113385155A CN202010173167.3A CN202010173167A CN113385155A CN 113385155 A CN113385155 A CN 113385155A CN 202010173167 A CN202010173167 A CN 202010173167A CN 113385155 A CN113385155 A CN 113385155A
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olefin
containing compound
adsorbent
cobalt
platinum
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曾海成
曾杰
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Dongguan Bingsheng Petrochemical Product Testing Co ltd
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Dongguan Bingsheng Petrochemical Product Testing Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
    • B01J20/282—Porous sorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/027—Compounds of F, Cl, Br, I
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/14—Diatomaceous earth
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/50—Aspects relating to the use of sorbent or filter aid materials
    • B01J2220/54—Sorbents specially adapted for analytical or investigative chromatography

Abstract

The invention discloses a reversible adsorbent for olefin content determination, a preparation method and application thereof, wherein the reversible adsorbent contains the following substances: a cobalt-containing compound, a platinum-containing compound, and a diatomaceous earth support. The preparation method comprises the following steps: dissolving cobalt-containing compound and platinum-containing compound in 80 deg.C deionized water, adding diatomite as carrier, heating while stirring to evaporate water to viscous state, and drying to obtain the final product. The reversible adsorbent can be used for preparing an olefin adsorption trap to adsorb olefin, or a gas chromatograph provided with the olefin adsorption trap. The reversible adsorbent has the advantage of higher trapping temperature, so that the penetration of low-carbon olefin and the adsorption of high-carbon saturated hydrocarbon are reduced when olefin is trapped.

Description

Reversible adsorbent for olefin content determination, and preparation method and application thereof
Technical Field
The invention relates to the field of olefin detection in gasoline, in particular to a reversible adsorbent for olefin content determination, a preparation method and application thereof.
Background
Gasoline is refined from petroleum and is mainly used as a fuel for spark-ignition internal combustion engines of automobiles. However, in the gasoline refining process, olefins are mixed in the gasoline inevitably. Because the olefin has obvious oxidation tendency, the olefin is easy to polymerize to form colloid, so that a gasoline nozzle is blocked, and carbon deposition is easy to form during combustion in an engine, so that the combustion efficiency of the engine is influenced. In addition, toxic diolefin is generated after the olefin is combusted, and pollutant emission is increased. Therefore, the olefin content of the gasoline needs to be controlled, and the olefin content of the produced gasoline needs to be detected in the production process.
When detecting the olefin content in gasoline, a gas chromatograph is generally adopted for detection, and an olefin adsorption trap is arranged in the gas chromatograph and can adsorb olefin. When in testing, the trapping temperature and the desorption temperature need to be set firstly, so that the temperature of the olefin adsorption trap reaches the trapping temperature, the olefin in the detected sample is adsorbed and trapped by the olefin adsorption trap and cannot escape, the peak area of the sample is detected (the olefin is removed), then the temperature of the olefin adsorption trap is raised to the desorption temperature, the olefin escapes from the olefin adsorption trap at the moment, the peak area of the sample is detected (the olefin is not removed), and then the content of the olefin in the gasoline is obtained by comparing the two data.
A commonly used olefin adsorption trap is made of quartz or stainless steel tubing with an adsorbent placed inside the tubing. At present, when the content of olefin in gasoline is detected, the used adsorbent is prepared by coating silver nitrate on the surface of a diatomite carrier. The olefins, when passing through the adsorbent, can be adsorbed and trapped by the silver nitrate-coated diatomaceous earth.
However, when the olefin adsorption trap adsorbs and traps olefins, the trapping temperature is generally 110 ℃ to 120 ℃, and in the temperature range, some high-carbon substances are also adsorbed and trapped by the adsorbent in the olefin adsorption trap, so that the content of olefins in the data is higher than the content of actual olefins, and the data is not accurate enough.
Disclosure of Invention
In view of the disadvantages of the prior art, the first object of the present invention is to provide a reversible adsorbent for olefin content determination, which has a higher collection temperature, so that the adsorption of high carbon saturated hydrocarbons is reduced when olefins are collected, and which can be reused many times.
The second purpose of the invention is to provide a preparation method of the reversible adsorbent for olefin content determination, which is used for preparing the reversible adsorbent.
The third objective of the present invention is to provide an olefin adsorption trap, which has high sensitivity for detecting the content of olefins in gasoline, and reduces the penetration of low carbon olefins and the adsorption of high carbon saturated hydrocarbons when capturing olefins, so that the detection is more accurate.
The fourth purpose of the invention is to provide a gas chromatograph, which has better accuracy in detecting the content of olefin in gasoline.
In order to achieve the first object, the invention provides the following technical scheme: a reversible adsorbent for olefin content determination contains the following substances: a cobalt-containing compound, a platinum-containing compound, and a diatomaceous earth support;
wherein the cobalt-containing compound contains cobalt element, the weight of the cobalt element accounts for 2.1-2.7% of the total weight of the reversible adsorbent, and the cobalt-containing compound is cobalt chloride;
wherein the platinum-containing compound comprises platinum element, the weight of the platinum element accounts for 1.1-1.9% of the total weight of the reversible adsorbent, and the platinum-containing compound is any one of potassium chloroplatinate, chloroplatinic acid or ammonium chloroplatinate;
the balance is diatomite carrier;
by adopting the technical scheme, when the olefin is adsorbed, the cobalt ions ionized from the cobalt-containing compound and the platinum ions ionized from the platinum-containing compound are utilized to carry out a complex reaction with the olefin to form chemical adsorption, so that the olefin is adsorbed in the adsorbent. At 110 ℃, the existing adsorbent added with silver nitrate can absorb more high-carbon saturated hydrocarbons while absorbing olefin in the adsorbent, so that the test is not accurate enough, and when the existing adsorbent is at 135 ℃, the olefin absorbed in the adsorbent can escape more, so that the test is not accurate enough. Cobalt chloride is easy to ionize cobalt ions and is not easy to react with substances in the gasoline to cause consumption, and any one of potassium chloroplatinate, chloroplatinic acid or ammonium chloroplatinate is easy to ionize platinum ions and is not easy to react with the substances in the gasoline to cause consumption. When the olefin is adsorbed, the adsorbent can be heated to 135 ℃, the olefin is adsorbed in the reversible adsorbent, and the high-carbon saturated hydrocarbon can be desorbed, so that only the olefin is adsorbed in the reversible adsorbent, and when the temperature of the reversible adsorbent is increased in desorption, the low-carbon olefin can be desorbed and escaped from the adsorbent when the temperature of the reversible adsorbent is 210-220 ℃, and the low-carbon olefin can be recycled, thereby realizing the reversible adsorption.
Further, the diatomite carrier is a red diatomite carrier.
By adopting the technical scheme, the red diatomite carrier has the advantages of small aperture, large specific surface area, high mechanical strength, small tailing effect and better effect in adsorbing and trapping olefin.
Further, the red diatomite carrier is a 6201 red diatomite carrier.
Further, the reversible adsorbent contains the following: the cobalt-containing compound contains cobalt element, the weight of the cobalt element accounts for 2.3% of the total weight of the reversible adsorbent, and the cobalt-containing compound is cobalt chloride;
the platinum-containing compound comprises platinum element, the weight of the platinum element accounts for 1.5% of the total weight of the reversible adsorbent, and the platinum-containing compound is any one of potassium chloroplatinate, chloroplatinic acid or ammonium chloroplatinate;
the balance is diatomite carrier;
by adopting the technical scheme, experiments show that when the weight of the cobalt element in the reversible adsorbent accounts for 2.3% of the total weight of the reversible adsorbent, and the weight of the platinum element accounts for 1.5% of the total weight of the reversible adsorbent, the adsorption effect of the adsorbent on olefin is good, and the adsorption on high-saturated alkane is reduced.
Further, cobalt chloride is cobalt chloride hexahydrate produced by alatin corporation.
Further, potassium chloroplatinate, chloroplatinic acid or ammonium chloroplatinate are all produced by the company Aladdin.
In order to achieve the second object, the invention provides the following technical scheme: a preparation method of a reversible adsorbent for olefin content determination comprises the following steps:
dissolving the cobalt-containing compound and the platinum-containing compound in deionized water at 70-90 ℃, adding a diatomite carrier, continuously heating and evaporating water under the stirring action to enable the mixture to be viscous, and then placing the materials in an oven at 210 ℃ of 190 ℃ for drying for 20-28 hours to obtain the product.
By adopting the technical scheme, the cobalt-containing compound and the platinum-containing compound are firstly put into deionized water for dissolving, then the diatomite carrier is added for uniformly mixing, then the water is evaporated, the mixture is viscous, and the mixture is dried to obtain a product with uniform distribution of the cobalt-containing compound and the platinum-containing compound.
Further, the cobalt-containing compound and the platinum-containing compound were dissolved in deionized water at 80 ℃.
By adopting the technical scheme, the cobalt-containing compound and the platinum-containing compound can be better dissolved by the deionized water at the temperature of 80 ℃, so that the cobalt-containing compound and the platinum-containing compound are more uniformly mixed.
Further, the drying temperature was 200 ℃.
Through adopting above-mentioned technical scheme, the stoving temperature can make dry product for 200 ℃, if the temperature is too high, can cause the waste of the energy, can cause the damage to the product moreover easily, if the temperature is lower, then the time that needs is longer when drying, if the temperature is low, then difficult stoving.
Further, when the mixture is viscous, the water content in the mixture is less than 10% when evaporating the water.
Through adopting above-mentioned technical scheme, when the mixture is thick, the moisture in the mixture is less, and the stoving time is shorter this moment, if the mixture moisture is more, the mixture need consume more time when the stoving, just stop heating if the mixture is drier, the mixture is burnt end easily, causes the waste.
In order to achieve the third object, the invention provides the following technical solutions: an olefin adsorption trap comprises a pipe body and the reversible adsorbent, wherein the reversible adsorbent is filled in the pipe body.
By adopting the technical scheme, the reversible adsorbent is filled in the tube body to form the olefin adsorbent, so that when the olefin is adsorbed, the gas containing the olefin can move from one end of the tube body to the other end, and the olefin is adsorbed by the olefin adsorption trap in the process.
Furthermore, the particle size range of the reversible adsorbent is 60-80 meshes.
By adopting the technical scheme, in the process of screening the reversible adsorbent, the reversible adsorbent can be firstly crushed, and then screened out by using a sieve with the particle size range of 60-80 meshes. When the particle size range of the reversible adsorbent is 60-80 meshes, the olefin adsorption trap has a good olefin adsorption effect, if the particle size of the reversible adsorbent is large, the adsorption effect is not good enough, and if the particle size of the reversible adsorbent is small, when gas passes through the olefin adsorption trap, the gas pressure in the olefin adsorption trap is large, so that the gas is not easy to pass through.
Further, the reversible adsorbent has an average particle size of 70 mesh.
Further, the body is stainless steel pipe body, and the size is 300mm 3 mm.
Through adopting above-mentioned technical scheme, the heating to the body when the nonrust steel pipe body can bear entrapment and desorption, and the body that the size is 300mm 3mm in addition carries out the adaptation with gas chromatograph that can be fine.
In order to achieve the fourth object, the invention provides the following technical solutions: a gas chromatograph includes a body and the olefin adsorption trap, the olefin adsorption trap is disposed within the body, and the olefin adsorption trap is used for trapping olefins.
By adopting the technical scheme, the olefin adsorption trap is arranged on the main body of the gas chromatograph, and the olefin adsorption trap can adsorb olefin when the gas chromatograph measures the content. When in test, the trapping temperature and the desorption temperature are set firstly, so that the temperature of the olefin adsorption trap reaches the trapping temperature, the olefin in the detected sample is adsorbed and trapped by the olefin adsorption trap and cannot escape, the peak area of the sample is detected (the olefin is removed), then the temperature of the olefin adsorption trap is raised to the desorption temperature, the olefin escapes from the olefin adsorption trap at the moment, the peak area of the sample is detected (the olefin is not removed), and then the content of the olefin in the gasoline is obtained by comparing the two data. After the temperature is raised to the desorption temperature, no olefin residue exists in the reversible adsorbent, so that when the olefin adsorption trap is cooled to the trapping temperature, the olefin adsorption trap can still adsorb olefin, and the gasoline can be repeatedly detected.
In conclusion, the invention has the following beneficial effects:
firstly, the reversible adsorbent adopts the cobalt-containing compound and the platinum-containing compound, and cobalt ions ionized by the cobalt-containing compound and the platinum-containing compound are complexed with olefin, so that the olefin is chemically adsorbed, the adsorption effect is good, the olefin can be adsorbed at a high temperature, the adsorption of high-carbon saturated hydrocarbon is effectively reduced, and the detection is more accurate when the olefin content in the gasoline is measured.
Secondly, the method of the invention dissolves the substances in the deionized water, and then evaporates and dries the substances to obtain the uniform reversible adsorbent, so the reversible adsorbent has better effect on the adsorption of the olefin.
Thirdly, the olefin adsorption trap of the invention has better adsorption effect when adsorbing olefin and can reduce the adsorption of high carbon saturated hydrocarbon because the reversible adsorbent prepared by the invention is contained in the olefin adsorption trap.
Fourthly, the gas chromatograph of the invention is more accurate in detecting the olefin content in the gasoline due to the application of the olefin adsorption trap prepared by the invention, can repeatedly detect the gasoline for many times and has higher cost performance.
Detailed Description
The present invention will be described in further detail with reference to examples and application examples.
Wherein the cobalt chloride is cobalt chloride hexahydrate produced by Allantin company;
the potassium chloroplatinate is produced by Aladdin company;
the chloroplatinic acid is produced by Aladdin company;
ammonium chloroplatinate produced by Aladdin company is selected.
Selecting an instrument: heating to evaporate water with commercially available electric heating plate, oven drying with commercially available oven, and sieving with commercially available mesh sieve.
Example 1
A reversible adsorbent for olefin content determination is prepared by the following method:
1.10g of cobalt chloride (the weight of cobalt element is 2.5% of the total weight of the reversible adsorbent) and 0.43g of chloroplatinic acid (the weight of platinum element is 1.5% of the total weight of the reversible adsorbent) were dissolved in 100ml of 80 ℃ deionized water, 9.47g of 6201 red diatomaceous earth was added, and water was evaporated by heating under stirring to a viscous state. Baking the mixture in an oven at 200 ℃ for 24 hours to obtain the adsorbent. Pulverizing adsorbent, sieving, collecting the part with particle size of 60 mesh and 80 mesh, and filling into 300mmx3mm stainless steel tube to obtain olefin adsorption trap.
Example 2
A reversible adsorbent for olefin content determination is prepared by the following method:
0.95g of cobalt chloride (the weight of cobalt element is 2.2% of the total weight of the reversible adsorbent) and 0.37g of ammonium chloroplatinate (the weight of platinum element is 1.5% of the total weight of the reversible adsorbent) were dissolved in 100ml of 80 ℃ deionized water, 9.68g of 6201 red diatomaceous earth was added, and water was evaporated by heating under stirring to a viscous state. Baking the mixture in an oven at 200 ℃ for 24 hours to obtain the adsorbent. Pulverizing adsorbent, sieving, collecting the part with particle size of 60 mesh and 80 mesh, and filling into 300mmx3mm stainless steel tube to obtain olefin adsorption trap.
Example 3
A reversible adsorbent for olefin content determination is prepared by the following method:
0.98g of cobalt chloride (the weight of cobalt element is 2.3% of the total weight of the reversible adsorbent) and 0.48g of chloroplatinic acid (the weight of platinum element is 1.7% of the total weight of the reversible adsorbent) were dissolved in 100ml of 80 ℃ deionized water, 9.54g of 6201 red diatomaceous earth was added, and water was evaporated by heating under stirring to a viscous state. Baking the mixture in an oven at 190 ℃ for 24 hours to obtain the adsorbent. Pulverizing adsorbent, sieving, collecting the part with particle size of 60 mesh and 80 mesh, and filling into 300mmx3mm stainless steel tube to obtain olefin adsorption trap.
Example 4
A reversible adsorbent for olefin content determination is prepared by the following method:
1.12g of cobalt chloride (the weight of cobalt element is 2.6% of the total weight of the reversible adsorbent) and 0.45g of ammonium chloroplatinate (the weight of platinum element is 1.8% of the total weight of the reversible adsorbent) were dissolved in 100ml of 80 ℃ deionized water, 9.43g of 6201 red diatomaceous earth was added, and water was evaporated by heating under stirring to a viscous state. And baking the mixture in an oven at the temperature of 210 ℃ for 24 hours to obtain the adsorbent. Pulverizing adsorbent, sieving, collecting the part with particle size of 60 mesh and 80 mesh, and filling into 300mmx3mm stainless steel tube to obtain olefin adsorption trap.
Example 5
A reversible adsorbent for olefin content determination is prepared by the following method:
1.17g of cobalt chloride (the weight of cobalt element is 2.7% of the total weight of the reversible adsorbent) and 0.29g of potassium chloroplatinate (the weight of platinum element is 1.1% of the total weight of the reversible adsorbent) were dissolved in 100ml of 80 ℃ deionized water, 9.54g of 6201 red diatomaceous earth was added, and water was evaporated by heating under stirring to a viscous state. Baking the mixture in an oven at 200 ℃ for 24 hours to obtain the adsorbent. Pulverizing adsorbent, sieving, collecting the part with particle size of 60 mesh and 80 mesh, and filling into 300mmx3mm stainless steel tube to obtain olefin adsorption trap.
Example 6
A reversible adsorbent for olefin content determination is prepared by the following method:
0.91g of cobalt chloride (the weight of cobalt element is 2.1% of the total weight of the reversible adsorbent) and 0.51g of potassium chloroplatinate (the weight of platinum element is 1.9% of the total weight of the reversible adsorbent) were dissolved in 100ml of 80 ℃ deionized water, 9.58g of 6201 red diatomaceous earth was added, and water was evaporated by heating under stirring to a viscous state. Baking the mixture in an oven at 200 ℃ for 24 hours to obtain the adsorbent. Pulverizing adsorbent, sieving, collecting the part with particle size of 60 mesh and 80 mesh, and filling into 300mmx3mm stainless steel tube to obtain olefin adsorption trap.
Example 7
A reversible adsorbent for olefin content determination is prepared by the following method:
1.00g of cobalt chloride (the weight of cobalt element is 2.3 percent of the total weight of the reversible adsorbent) and 0.40g of potassium chloroplatinate (the weight of platinum element is 1.5 percent of the total weight of the reversible adsorbent) were dissolved in 100ml of deionized water at 80 ℃, 9.60g of 6201 red diatomite was added, and water was evaporated by heating under stirring to be viscous. Baking the mixture in an oven at 200 ℃ for 24 hours to obtain the adsorbent. Pulverizing adsorbent, sieving, collecting the part with particle size of 60 mesh and 80 mesh, and filling into 300mmx3mm stainless steel tube to obtain olefin adsorption trap.
Example 8
Example 8 differs from example 7 in that the adsorbent was crushed and sieved, and a portion between 30 mesh and 50 mesh was packed in a stainless steel tube of 300mmx3mm to prepare an olefin adsorption trap.
Example 9
Example 9 differs from example 7 in that the adsorbent was crushed and sieved, and then a portion between 100 mesh and 120 mesh was packed in a stainless steel tube of 300mmx3mm to prepare an olefin adsorption trap.
Example 10
A gas chromatograph comprises a main body and an olefin adsorption trap, wherein the main body is selected from the prior art, in the embodiment, the main body is an Shimadzu GC14A gas chromatograph, the olefin adsorption trap is mounted on the main body, and the olefin adsorption trap is selected from the prior art and can be connected through a connection mode such as a threaded connection.
Comparative example 1
1.40g of silver nitrate (elemental silver accounting for 3.8% by weight of the total weight of the reversible adsorbent) was dissolved in 100ml of 80 ℃ deionized water, 9.60g of 6201 red diatomaceous earth was added, and the water was evaporated by heating under stirring to a viscous state. And (5) baking the mixture in an oven at the temperature of 200 ℃ for 24 hours to obtain the product. Then taking out the product, crushing and sieving, and filling the part between 60 meshes and 80 meshes in a stainless steel pipe with the size of 300mmx3mm to prepare an olefin adsorption trap.
Comparative example 2
1.00g of cobalt chloride (the weight of cobalt element is 2.3% of the total weight of the reversible adsorbent) was dissolved in 100ml of 80 ℃ deionized water, 10.00g of 6201 red diatomaceous earth was added, and the water was evaporated by heating under stirring to a viscous state. And (5) baking the mixture in an oven at the temperature of 200 ℃ for 24 hours to obtain the product. Then taking out the product, crushing and sieving, and filling the part between 60 meshes and 80 meshes in a stainless steel pipe with the size of 300mmx3mm to prepare an olefin adsorption trap.
Comparative example 3
1.65g of cobalt chloride (the weight of cobalt element amounting to 3.8% of the total weight of the reversible adsorbent) was dissolved in 100ml of 80 ℃ deionized water, 9.35g of 6201 red diatomaceous earth was added, and the water was evaporated by heating under stirring to a viscous state. And (5) baking the mixture in an oven at the temperature of 200 ℃ for 24 hours to obtain the product. Then taking out the product, crushing and sieving, and filling the part between 60 meshes and 80 meshes in a stainless steel pipe with the size of 300mmx3mm to prepare an olefin adsorption trap.
Comparative example 4
0.40g of potassium chloroplatinate (1.5% by weight of the platinum element based on the total weight of the reversible adsorbent) was dissolved in 100ml of 80 ℃ deionized water, 10.60g of 6201 red diatomaceous earth was added, and the water was evaporated by heating under stirring to a viscous state. And (5) baking the mixture in an oven at the temperature of 200 ℃ for 24 hours to obtain the product. Then taking out the product, crushing and sieving, and filling the part between 60 meshes and 80 meshes in a stainless steel pipe with the size of 300mmx3mm to prepare an olefin adsorption trap.
Comparative example 5
1.01g of potassium chloroplatinate (the weight of the platinum element amounting to 3.8% of the total weight of the reversible adsorbent) was dissolved in 100ml of 80 ℃ deionized water, 9.99g of 6201 red diatomaceous earth was added, and the water was evaporated by heating under stirring to a viscous state. And (5) baking the mixture in an oven at the temperature of 200 ℃ for 24 hours to obtain the product. Then taking out the product, crushing and sieving, and filling the part between 60 meshes and 80 meshes in a stainless steel pipe with the size of 300mmx3mm to prepare an olefin adsorption trap.
Performance test
The detection is carried out by adopting the detection standard of GB/T30519-2016.
The detection adopts an instrument: shimadzu GC14A gas chromatograph, Kekedi BCEF column, Lanzhou, 25mx0.53mmx2.5 μm DB-1 column, olefin adsorption trap prepared in examples 1-9 and comparative examples 1-5.
1. The olefin adsorption traps prepared in examples 1 to 9 and comparative examples 1 to 5 were respectively installed on the same gas chromatograph (Shimadzu GC14A gas chromatograph) to prepare application examples 1 to 9 and comparative application examples 1 to 5 in this order, with the trapping temperature set at 135 deg.C, the desorption temperature set at 210 deg.C, and the sample introduction amount set at 1. mu.L. The peak area when no more than one olefin was adsorbed to the trap and the peak area when more than one olefin was adsorbed to the trap were then measured by passing 1-pentene (25%) and n-tetradecane (5%), respectively, and each set was measured 5 times, and the average peak areas were taken, and the data are shown in Table 1.
Figure BDA0002409894420000081
TABLE 1
2. The olefin adsorption traps prepared in examples 1 to 9 and comparative examples 1 to 5 were respectively mounted on the same gas chromatograph (Shimadzu GC14A gas chromatograph) to prepare application examples 1 to 9 and comparative application examples 1 to 5, where the trapping temperature was set to 135 ℃, the desorption temperature was set to 210 ℃, and the sample introduction amount was 1. mu.L. The peak area when no more than olefin was adsorbed to the trap and the peak area when more than olefin was adsorbed to the trap were then separately passed through ethylene (25%), and each group was tested 5 times to obtain the average peak area, and the data are shown in Table 2.
Figure BDA0002409894420000091
TABLE 2
3. The olefin adsorption trap prepared in example 7 was installed on a gas chromatograph (shimadzu GC14A gas chromatograph) and the trapping temperatures were all set to 135 c, the desorption temperatures were all set to 210 c, and the sample volumes were all 1 μ L. The peak area when no more than the olefin was adsorbed in the trap and the peak area when more than the olefin was adsorbed in the trap were continuously measured 5 times by passing 1-pentene (25%) and n-tetradecane (5%), respectively, and the data are shown in Table 3.
Figure BDA0002409894420000101
TABLE 3
Note: 1. however, since the peak area of the olefin adsorption well was measured, no sample gas passed through the olefin adsorption well, no substance was adsorbed by the olefin adsorption well, and this was used as reference blank comparative data.
2. When the peak area of the over-olefin adsorption trap is measured, the sample gas passes through the olefin adsorption trap, and part of substances are adsorbed by the olefin adsorption trap, so that the peak area is smaller than that of the over-olefin adsorption trap, and the difference part is the peak area of the substances adsorbed by the olefin adsorption trap.
3. The larger the peak area, the more the content of the substance.
As can be seen from tables 1 and 2, in application examples 1 to 7, when the olefin adsorption trap was prepared in the manner of example 7, the olefin adsorption trap adsorbed less 1-pentene and less n-tetradecane, so that the olefin adsorption trap did not adsorb more high-carbon saturated hydrocarbons when adsorbing olefins, and thus the data was more accurate when olefin measurement was performed on gasoline. Because the alkane with lower carbon number is more easily absorbed by the alkane adsorption trap than the alkane with higher carbon number and the carbon number of the n-tetradecane is lower under the same temperature, when the alkane is actually measured on the gasoline, the high-carbon saturated alkane absorbed by the alkene adsorption trap is less, and the result of measuring the alkene content is more accurate.
As can be seen from tables 1 and 2, the comparison between application examples 1-4 and application examples 5-7 shows that the platinum-containing compound is better in selecting potassium chloroplatinate, and the obtained olefin adsorption trap has better effect.
As can be seen from tables 1 and 2, it is better to select a reversible adsorption trap with a mesh size in the range of 60 to 80 mesh when manufacturing an olefin adsorption trap in application example 7 in comparison with application examples 8 and 9.
As can be seen from table 2, when application examples 1 to 7 are compared with comparative application example 1, at 135 ℃, the olefin adsorption trap prepared in the prior art at present has an insufficient olefin adsorption effect, and low-carbon olefins are easy to penetrate due to too high temperature, so that the low-carbon olefins grabbing capacity is reduced. As can be seen from Table 1, the comparison of application examples 1-7 with comparative application example 1 shows that the olefin adsorption traps prepared in examples 1-7 adsorb less high carbon saturated hydrocarbons. The data is more accurate when the olefin content in gasoline is measured using the olefin adsorption traps prepared in examples 1-7.
As can be seen from tables 1 and 2, the results of the comparison of application examples 1 to 7 with comparative application example 2 and comparative application example 3 are far less effective than those of the olefin trap containing both compounds when only the cobalt-containing compound is present. Indicating that the olefin adsorption trap comprising both a cobalt-containing compound and a platinum-containing compound is more accurate in the determination.
As can be seen from tables 1 and 2, the results of the comparison of application examples 1 to 7 with comparative application examples 4 and 5 are far less effective than the olefin trap containing both compounds when only the platinum-containing compound is present. Indicating that the olefin adsorption trap comprising both a cobalt-containing compound and a platinum-containing compound is more accurate in the determination.
As can be seen from table 3, when the measurements were continuously performed 5 times, the fluctuation value of the measurements was not large, indicating that the adsorption trap is a reversible adsorption trap, and can be recycled, and the effect of the adsorption trap will not be deteriorated by recycling.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.

Claims (10)

1. A reversible adsorbent for olefin content determination, comprising: a cobalt-containing compound, a platinum-containing compound, and a diatomaceous earth support;
wherein the cobalt-containing compound comprises cobalt element, the weight of the cobalt element accounts for 2.1-2.7% of the total weight of the reversible adsorbent, and the cobalt-containing compound is cobalt chloride;
wherein the platinum-containing compound comprises platinum element, the weight of the platinum element accounts for 1.1-1.9% of the total weight of the reversible adsorbent, and the platinum-containing compound is any one of potassium chloroplatinate, chloroplatinic acid or ammonium chloroplatinate;
the balance is diatomite carrier.
2. The reversible adsorbent for olefin content determination according to claim 1, wherein the diatomaceous earth support is red diatomaceous earth support.
3. The reversible adsorbent for olefin content determination according to claim 1, wherein the cobalt-containing compound comprises cobalt element, the weight of the cobalt element is 2.3% of the total weight of the reversible adsorbent, and the cobalt-containing compound is cobalt chloride;
the platinum-containing compound comprises platinum element, the weight of the platinum element accounts for 1.5% of the total weight of the reversible adsorbent, and the platinum-containing compound is any one of potassium chloroplatinate, chloroplatinic acid or ammonium chloroplatinate;
the balance is diatomite carrier.
4. A method for preparing a reversible adsorbent for olefin content measurement, which is used for preparing the reversible adsorbent for olefin content measurement according to any one of claims 1 to 3, and comprises the following steps:
dissolving the cobalt-containing compound and the platinum-containing compound in deionized water at 70-90 ℃, adding a diatomite carrier, continuously heating and evaporating water under the stirring action to enable the mixture to be viscous, and then placing the materials in an oven at 210 ℃ of 190 ℃ for drying for 20-28 hours to obtain the product.
5. The method for preparing the reversible adsorbent for olefin content determination according to claim 4, wherein the cobalt-containing compound and the platinum-containing compound are dissolved in deionized water at 80 ℃.
6. The method for preparing the reversible adsorbent for olefin content determination according to claim 5, wherein the drying temperature is 200 ℃.
7. An olefin adsorption trap made of the reversible adsorbent for olefin content determination according to claims 1 to 6, comprising a tube and the reversible adsorbent, wherein the reversible adsorbent is filled in the tube.
8. The olefin adsorption trap of claim 7, wherein the reversible adsorbent has a particle size in the range of 60 to 80 mesh.
9. An olefin adsorption trap as claimed in claim 8, wherein said tube is a stainless steel tube and has a dimension of 300mm x3 mm.
10. A gas chromatograph comprising an olefin adsorption trap as defined in any of claims 7 to 9.
CN202010173167.3A 2020-03-13 2020-03-13 Reversible adsorbent for olefin content determination, and preparation method and application thereof Pending CN113385155A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030097933A1 (en) * 2001-11-23 2003-05-29 Indian Petrochemicals Corporation Limited Adsorbents, method for the manufacture thereof and process for the separation of unsaturated hydrocarbons from gas mixture
CN1485129A (en) * 2002-09-28 2004-03-31 中国石油化工股份有限公司 Adsorbing material and the application thereof
CN1621830A (en) * 2003-11-28 2005-06-01 中国石油化工股份有限公司 Method for analyzing composition of alcohol-containing gasoline and alcohol adsorption material used thereby
CN101519602A (en) * 2008-02-28 2009-09-02 中国石油化工股份有限公司 Material for trapping the unsaturated hydrocarbon in hydrocarbon raw materials

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030097933A1 (en) * 2001-11-23 2003-05-29 Indian Petrochemicals Corporation Limited Adsorbents, method for the manufacture thereof and process for the separation of unsaturated hydrocarbons from gas mixture
CN1485129A (en) * 2002-09-28 2004-03-31 中国石油化工股份有限公司 Adsorbing material and the application thereof
CN1621830A (en) * 2003-11-28 2005-06-01 中国石油化工股份有限公司 Method for analyzing composition of alcohol-containing gasoline and alcohol adsorption material used thereby
CN101519602A (en) * 2008-02-28 2009-09-02 中国石油化工股份有限公司 Material for trapping the unsaturated hydrocarbon in hydrocarbon raw materials

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