Efficient complex iron desulfurizer as well as preparation method and application thereof

Abstract

The invention relates to the technical field of desulfurization, and provides an efficient complex iron desulfurizer as well as a preparation method and application thereof, and the desulfurizer comprises the following components in parts by weight: 25-80 parts of ferric tartrate, 5-20 parts of ferric ethylene diamine tetraacetate, 10-20 parts of an absorbent, 5-20 parts of a stabilizer, 20-30 parts of a synergist and 500-1000 parts of water. According to the technical scheme, the problem of low desulfurization efficiency of a desulfurizing agent in related technologies is solved.

Description

Technical Field

[0001] The invention relates to the technical field of desulfurization, and in particular to a high-efficiency complex iron desulfurizer and a preparation method and application thereof. Background Art

[0002] Under standard conditions, H2S is a flammable acidic gas that is colorless and has the smell of rotten eggs at low concentrations. It plays multiple roles in nature and human industrial activities, with unique properties, hazards that cannot be ignored, and diverse practical uses.

[0003] In the industrial field, hydrogen sulfide has multiple application values. In oil and natural gas extraction, it exists in large quantities as an associated gas. Accurate detection of its content is crucial to evaluating the quality of oil and gas reservoirs and optimizing the extraction process. However, long-term exposure can irritate the respiratory tract, causing uncomfortable symptoms such as coughing, stinging eyes, and tearing, leading to frequent respiratory inflammation. The harm of hydrogen sulfide to organisms is serious, so H2S removal technology is highly valued.

[0004] In order to improve the removal efficiency of H2S, new desulfurizers have been continuously studied and disclosed in recent years, but the desulfurization efficiency of most desulfurizers is not high. Therefore, it is of great significance to study a desulfurizer with good desulfurization performance. Summary of the invention

[0005] The invention provides a high-efficiency complex iron desulfurizer and a preparation method and application thereof, which solves the problem of low desulfurization efficiency in the related art.

[0006] The technical solution of the present invention is as follows: The invention provides a high-efficiency complex iron desulfurizer, which comprises the following components in parts by weight: 25-80 parts of ferric tartrate, 5-20 parts of ethylenediaminetetraacetic acid ferric, 10-20 parts of an absorbent, 5-20 parts of a stabilizer, 20-30 parts of a synergist, and 500-1000 parts of water.

[0007] As a further technical solution, the weight ratio of the ferric tartrate to ferric ethylenediaminetetraacetate is 3-5:1.

[0008] When the weight ratio of ferric tartrate to ferric ethylenediaminetetraacetate is 3-5:1, the desulfurization efficiency of the desulfurizer is further improved.

[0009] As a further technical solution, the weight ratio of the ferric tartrate to ferric ethylenediaminetetraacetate is 4:1.

[0010] When the weight ratio of ferric tartrate to ferric ethylenediaminetetraacetate is 4:1, the desulfurization efficiency of the desulfurizer is further improved.

[0011] As a further technical solution, the absorbent includes one or both of pyridine and pyrrole.

[0012] The absorbent can react with hydrogen sulfide to generate hydrogen sulfide anions, thereby increasing the reaction rate of the desulfurization reaction.

[0013] As a further technical solution, the stabilizer includes one or more of 3-butene-1-amine, diallylamine, and pent-4-ene-1-amine.

[0014] The double bonds in the stabilizer serve to capture hydroxyl radicals, thereby slowing down the degradation of the organic complex.

[0015] As a further technical solution, when the stabilizer is 3-butene-1-amine and diallylamine, the weight ratio of the 3-butene-1-amine to diallylamine is 1-3:1.

[0016] When the stabilizer is 3-butene-1-amine and diallylamine, the two produce a synergistic effect to further improve the desulfurization efficiency, and when the weight ratio of 3-butene-1-amine and diallylamine is 1~3:1, the desulfurization efficiency of the desulfurizer can be further improved.

[0017] As a further technical solution, when the stabilizer is 3-butene-1-amine and diallylamine, the weight ratio of the 3-butene-1-amine to diallylamine is 2:1.

[0018] When the weight ratio of 3-butene-1-amine to diallylamine is 2:1, the desulfurization efficiency of the desulfurizer can be further improved.

[0019] As a further technical solution, the synergist includes one or more of hydroquinone, piperazine, and sulfolane.

[0020] The present invention also provides a method for preparing the highly efficient complex iron desulfurizer, which comprises the following steps: uniformly mixing the components to obtain the desulfurizer.

[0021] The present invention also proposes the application of the high-efficiency complex iron desulfurizer or the desulfurizer prepared by the preparation method in the field of desulfurization technology.

[0022] The working principle and beneficial effects of the present invention are: In the present invention, both ferric tartrate and ferric ethylenediaminetetraacetate are iron complexing agents, and ferric tartrate can produce a synergistic effect with ferric ethylenediaminetetraacetate, thereby improving the selectivity of the reaction and thus improving the desulfurization efficiency. DETAILED DESCRIPTION

[0023] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] Example 1 A highly efficient complex iron desulfurizer comprises the following components in parts by weight: 25 parts of ferric tartrate, 5 parts of ethylenediaminetetraacetic acid iron, 10 parts of pyridine, 5 parts of 3-butene-1-amine, 20 parts of hydroquinone, and 500 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0025] Example 2 A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 52 parts of ferric tartrate, 8 parts of ethylenediaminetetraacetic acid iron, 15 parts of pyridine, 12 parts of 3-butene-1-amine, 25 parts of hydroquinone, and 800 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0026] Example 3 A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 80 parts of ferric tartrate, 20 parts of ethylenediaminetetraacetic acid iron, 20 parts of pyridine, 20 parts of 3-butene-1-amine, 30 parts of hydroquinone, and 1000 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0027] Example 4 A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 40 parts of ferric tartrate, 20 parts of ferrous ethylenediaminetetraacetate, 15 parts of pyridine, 12 parts of 3-butene-1-amine, 25 parts of hydroquinone, and 800 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0028] Example 5 A highly efficient complex iron desulfurizer comprises the following components in parts by weight: 45 parts of ferric tartrate, 15 parts of ferrous ethylenediaminetetraacetate, 15 parts of pyridine, 12 parts of 3-butene-1-amine, 25 parts of hydroquinone, and 800 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0029] Example 6 A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 48 parts of ferric tartrate, 12 parts of ethylenediaminetetraacetic acid iron, 15 parts of pyridine, 12 parts of 3-butene-1-amine, 25 parts of hydroquinone, and 800 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0030] Example 7 A highly efficient complex iron desulfurizer comprises the following components in parts by weight: 50 parts of ferric tartrate, 10 parts of ferrous ethylenediaminetetraacetate, 15 parts of pyridine, 12 parts of 3-butene-1-amine, 25 parts of hydroquinone, and 800 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0031] Example 8 A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 48 parts of ferric tartrate, 12 parts of ethylenediaminetetraacetic acid iron, 15 parts of pyridine, 12 parts of diallylamine, 25 parts of hydroquinone, and 800 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0032] Example 9 A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 48 parts of ferric tartrate, 12 parts of ethylenediaminetetraacetic acid iron, 15 parts of pyridine, 12 parts of pent-4-en-1-amine, 25 parts of hydroquinone, and 800 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0033] Example 10 A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 48 parts of ferric tartrate, 12 parts of ethylenediaminetetraacetic acid iron, 15 parts of pyridine, 4 parts of 3-butene-1-amine, 8 parts of diallylamine, 25 parts of hydroquinone, and 800 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0034] Embodiment 11 A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 48 parts of ferric tartrate, 12 parts of ethylenediaminetetraacetic acid iron, 15 parts of pyridine, 10 parts of 3-butene-1-amine, 2 parts of diallylamine, 25 parts of hydroquinone, and 800 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0035] Example 12 A highly efficient complex iron desulfurizer comprises the following components in parts by weight: 48 parts of ferric tartrate, 12 parts of ethylenediaminetetraacetic acid iron, 15 parts of pyridine, 6 parts of 3-butene-1-amine, 6 parts of diallylamine, 25 parts of hydroquinone, and 800 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0036] Example 13 A highly efficient complex iron desulfurizer comprises the following components in parts by weight: 48 parts of ferric tartrate, 12 parts of ethylenediaminetetraacetic acid iron, 15 parts of pyridine, 8 parts of 3-butene-1-amine, 4 parts of diallylamine, 25 parts of hydroquinone, and 800 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0037] Embodiment 14 A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 48 parts of ferric tartrate, 12 parts of ethylenediaminetetraacetic acid iron, 15 parts of pyridine, 9 parts of 3-butene-1-amine, 3 parts of diallylamine, 25 parts of hydroquinone, and 800 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0038] Comparative Example 1 A highly efficient complex iron desulfurizer comprises the following components in parts by weight: 30 parts of iron tartrate, 10 parts of pyridine, 5 parts of 3-butene-1-amine, 20 parts of hydroquinone, and 500 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0039] Comparative Example 2 A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 30 parts of ethylenediaminetetraacetic acid iron, 10 parts of pyridine, 5 parts of 3-butene-1-amine, 20 parts of hydroquinone, and 500 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0040] Comparative Example 3 A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 25 parts of ferric citrate, 5 parts of ethylenediaminetetraacetic acid iron, 10 parts of pyridine, 5 parts of 3-butene-1-amine, 20 parts of hydroquinone, and 500 parts of water; The preparation method comprises the following steps: mixing the components uniformly to obtain a desulfurizing agent.

[0041] Experimental example Desulfurization process: After the hydrogen sulfide gas is pressurized by the booster fan, it contacts the desulfurizer from the bottom to the top in the desulfurization tower in reverse order for desulfurization, and then passes through the demister at the top of the desulfurization tower for gas-water separation. The gas after the droplets are separated is discharged from the top outlet of the desulfurization tower and enters the next gas-using section; The desulfurizing agents prepared in Examples 1 to 14 and Comparative Examples 1 to 3 were subjected to desulfurization reaction by the above desulfurization process, and the specific operating parameters were controlled as follows: Inlet gas hydrogen sulfide volume fraction C1: 5000ppm (the rest is N2); inlet gas flow rate: 0.60L / min; air flow rate: 1.25L / min; temperature: 30℃; test time: 12h; total volume of desulfurizer solution: 10L; Calculation of desulfurization efficiency (K): K = (C1-C2) / C1×100%; the result is retained to 4 decimal places, where C1 and C2 represent the volume fraction of hydrogen sulfide in the inlet gas and the outlet gas, respectively; GB / T 11060.11-2014 "Determination of sulfur compounds in natural gas Part 11: Determination of hydrogen sulfide content by colored length detection tube method" is used to detect the volume fraction C2 of hydrogen sulfide in the outlet gas. The test results are shown in Table 1 below.

[0042] Table 1 Desulfurization test results

[0043] Compared with Comparative Examples 1 to 3, the desulfurization efficiency of Example 1 is significantly improved, indicating that ferric tartrate can produce a synergistic effect with ferric ethylenediaminetetraacetate, and the desulfurization efficiency can be significantly improved. Compared with Examples 2 and 4, the desulfurization efficiency of Examples 5 to 7 is significantly improved, indicating that when the ratio of ferric tartrate to ferric ethylenediaminetetraacetate is 3 to 5: 1, the desulfurization efficiency can be further improved. The desulfurization efficiency of Example 6 is greater than that of Examples 5 and 7, which indicates that when the ratio of ferric tartrate to ferric ethylenediaminetetraacetate is 4: 1, the desulfurization efficiency can be further improved; Compared with Examples 6 and 8 to 9, the desulfurization efficiency of Examples 10 to 14 is further improved, indicating that 3-butene-1-amine can produce a synergistic effect with diallylamine, and the desulfurization efficiency can be further improved. The desulfurization efficiency of Examples 12 to 14 is greater than that of Examples 10 to 11, indicating that when the ratio of 3-butene-1-amine to diallylamine is 1 to 3: 1, the desulfurization efficiency can be further improved. The desulfurization efficiency of Example 13 is greater than that of Examples 11 and 12, which indicates that the desulfurization efficiency is better when the ratio of 3-butene-1-amine to diallylamine is 2:1.

[0044] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A highly efficient complex iron desulfurizer, characterized in that: The invention comprises the following components in parts by weight: 25-80 parts of ferric tartrate, 5-20 parts of ethylenediaminetetraacetic acid ferric, 10-20 parts of absorbent, 5-20 parts of stabilizer, 20-30 parts of synergist and 500-1000 parts of water.

2. A highly efficient complex iron desulfurizer according to claim 1, characterized in that: The weight ratio of the ferric tartrate to ferric ethylenediaminetetraacetate is 3-5:

1.

3. A highly efficient complex iron desulfurizer according to claim 2, characterized in that: The weight ratio of the ferric tartrate to ferric ethylenediaminetetraacetate is 4:

1.

4. A highly efficient complex iron desulfurizer according to claim 1, characterized in that: The absorbent includes one or both of pyridine and pyrrole.

5. A highly efficient complex iron desulfurizer according to claim 1, characterized in that: The stabilizer includes one or more of 3-butene-1-amine, diallylamine, and pent-4-ene-1-amine.

6. A high-efficiency complex iron desulfurizer according to claim 5, characterized in that: When the stabilizer is 3-butene-1-amine and diallylamine, the weight ratio of the 3-butene-1-amine to diallylamine is 1-3:

1.

7. A high-efficiency complex iron desulfurizer according to claim 6, characterized in that: When the stabilizer is 3-butene-1-amine and diallylamine, the weight ratio of the 3-butene-1-amine to diallylamine is 2:

1.

8. A high-efficiency complex iron desulfurizer according to claim 1, characterized in that: The synergist includes one or more of hydroquinone, piperazine and sulfolane.

9. The method for preparing a high-efficiency complex iron desulfurizer according to any one of claims 1 to 8, characterized in that: The following steps are involved: The components are mixed uniformly to obtain the desulfurizing agent.

10. Use of the high-efficiency complex iron desulfurizer according to any one of claims 1 to 8 or the desulfurizer prepared by the preparation method according to claim 9 in the field of desulfurization technology.

Images