A high-efficiency complex iron desulfurizer and its preparation method and application
By preparing an efficient complex iron desulfurization agent, the synergistic effect of iron tartrate and iron ethylenediaminetetraacetate and combined with absorbents and stabilizers, the problem of low efficiency of existing desulfurization agents is solved, and the effect of efficient removal of hydrogen sulfide gas is achieved.
Patent Information
- Application Number
- CN202411831369.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-12
- Publication Date
- 2025-08-22
- Estimated Expiration
- 2044-12-12
AI Technical Summary
The desulfurization efficiency of existing desulfurization agents is not high, and it is difficult to effectively remove the large amount of hydrogen sulfide gases present in the industry.
High-efficiency complex iron desulfurization agent is used, consisting of iron tartrate, iron ethylenediaminetetraacetate, absorbent, stabilizer and synergist. Through specific proportions, a synergistic effect is formed to improve the desulfurization reaction efficiency.
It significantly improves the desulfurization efficiency, can efficiently remove hydrogen sulfide gas, reduces the harm to biological diseases, and is suitable for accurate detection and removal in oil and natural gas mining.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of desulfurization, and in particular to a high-efficiency complex iron desulfurizer, a preparation method thereof and an application thereof. Background Art
[0002] H2S is a flammable, colorless, acidic gas under standard conditions, with a rotten egg odor at low concentrations. It plays multiple roles in nature and in human industrial activities, possessing unique properties, significant hazards, 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 for evaluating the quality of oil and gas reservoirs and optimizing extraction processes. 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] To improve the removal efficiency of H2S, new desulfurizers have been continuously researched and released in recent years. However, 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 present invention provides a high-efficiency complex iron desulfurizer and a preparation method and application thereof, which solves the problem of low desulfurization efficiency in related technologies.
[0006] The technical solutions of the present invention are as follows:
[0007] 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 ferric ethylenediaminetetraacetate, 10-20 parts of an absorbent, 5-20 parts of a stabilizer, 20-30 parts of a synergist, and 500-1000 parts of water.
[0008] As a further technical solution, the weight ratio of the ferric tartrate to ferric ethylenediaminetetraacetate is 3-5:1.
[0009] When the weight ratio of ferric tartrate to ferric ethylenediaminetetraacetate is 3-5:1, the desulfurization efficiency of the desulfurizer is further improved.
[0010] As a further technical solution, the weight ratio of the ferric tartrate to ferric ethylenediaminetetraacetate is 4:1.
[0011] When the weight ratio of ferric tartrate to ferric ethylenediaminetetraacetate is 4:1, the desulfurization efficiency of the desulfurizer is further improved.
[0012] As a further technical solution, the absorbent includes one or both of pyridine and pyrrole.
[0013] The absorbent can react with hydrogen sulfide to generate hydrogen sulfide anions, thereby increasing the reaction rate of the desulfurization reaction.
[0014] As a further technical solution, the stabilizer includes one or more of 3-butene-1-amine, diallylamine, and pent-4-ene-1-amine.
[0015] The double bonds in the stabilizer serve to capture hydroxyl radicals, thereby slowing down the degradation of the organic complex.
[0016] 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 to 3:1.
[0017] When the stabilizers are 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.
[0018] 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.
[0019] When the weight ratio of 3-butene-1-amine to diallylamine is 2:1, the desulfurization efficiency of the desulfurizer can be further improved.
[0020] As a further technical solution, the synergist includes one or more of hydroquinone, piperazine, and sulfolane.
[0021] The present invention also provides a method for preparing the high-efficiency complex iron desulfurizer, which comprises the following steps: uniformly mixing the components to obtain the desulfurizer.
[0022] 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.
[0023] The working principle and beneficial effects of the present invention are:
[0024] In the present invention, both ferric tartrate and ferric ethylenediaminetetraacetate are iron complexing agents. At the same time, 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
[0025] 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 embodiments described 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 making any creative efforts are within the scope of protection of the present invention.
[0026] Example 1
[0027] A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 25 parts of ferric tartrate, 5 parts of ferric ethylenediaminetetraacetate, 10 parts of pyridine, 5 parts of 3-butene-1-amine, 20 parts of hydroquinone, and 500 parts of water;
[0028] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0029] Example 2
[0030] A high-efficiency complex iron desulfurizer, comprising the following components in parts by weight: 52 parts of ferric tartrate, 8 parts of ferric ethylenediaminetetraacetate, 15 parts of pyridine, 12 parts of 3-butene-1-amine, 25 parts of hydroquinone, and 800 parts of water;
[0031] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0032] Example 3
[0033] A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 80 parts of ferric tartrate, 20 parts of ferric ethylenediaminetetraacetate, 20 parts of pyridine, 20 parts of 3-butene-1-amine, 30 parts of hydroquinone, and 1000 parts of water;
[0034] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0035] Example 4
[0036] A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 40 parts of ferric tartrate, 20 parts of ferric ethylenediaminetetraacetate, 15 parts of pyridine, 12 parts of 3-butene-1-amine, 25 parts of hydroquinone, and 800 parts of water;
[0037] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0038] Example 5
[0039] A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 45 parts of ferric tartrate, 15 parts of ferric ethylenediaminetetraacetate, 15 parts of pyridine, 12 parts of 3-butene-1-amine, 25 parts of hydroquinone, and 800 parts of water;
[0040] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0041] Example 6
[0042] A high-efficiency complex iron desulfurizer, comprising the following components in parts by weight: 48 parts of ferric tartrate, 12 parts of ferric ethylenediaminetetraacetate, 15 parts of pyridine, 12 parts of 3-butene-1-amine, 25 parts of hydroquinone, and 800 parts of water;
[0043] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0044] Example 7
[0045] A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 50 parts of ferric tartrate, 10 parts of ferric ethylenediaminetetraacetate, 15 parts of pyridine, 12 parts of 3-butene-1-amine, 25 parts of hydroquinone, and 800 parts of water;
[0046] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0047] Example 8
[0048] A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 48 parts of ferric tartrate, 12 parts of ferric ethylenediaminetetraacetate, 15 parts of pyridine, 12 parts of diallylamine, 25 parts of hydroquinone, and 800 parts of water;
[0049] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0050] Example 9 A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 48 parts of ferric tartrate, 12 parts of ferric ethylenediaminetetraacetate, 15 parts of pyridine, 12 parts of pent-4-en-1-amine, 25 parts of hydroquinone, and 800 parts of water;
[0051] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0052] Example 10
[0053] A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 48 parts of ferric tartrate, 12 parts of ferric ethylenediaminetetraacetate, 15 parts of pyridine, 4 parts of 3-butene-1-amine, 8 parts of diallylamine, 25 parts of hydroquinone, and 800 parts of water;
[0054] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0055] Example 11
[0056] A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 48 parts of ferric tartrate, 12 parts of ferric ethylenediaminetetraacetate, 15 parts of pyridine, 10 parts of 3-butene-1-amine, 2 parts of diallylamine, 25 parts of hydroquinone, and 800 parts of water;
[0057] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0058] Example 12
[0059] A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 48 parts of ferric tartrate, 12 parts of ferric ethylenediaminetetraacetate, 15 parts of pyridine, 6 parts of 3-butene-1-amine, 6 parts of diallylamine, 25 parts of hydroquinone, and 800 parts of water;
[0060] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0061] Example 13
[0062] A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 48 parts of ferric tartrate, 12 parts of ferric ethylenediaminetetraacetate, 15 parts of pyridine, 8 parts of 3-butene-1-amine, 4 parts of diallylamine, 25 parts of hydroquinone, and 800 parts of water;
[0063] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0064] Example 14
[0065] A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 48 parts of ferric tartrate, 12 parts of ferric ethylenediaminetetraacetate, 15 parts of pyridine, 9 parts of 3-butene-1-amine, 3 parts of diallylamine, 25 parts of hydroquinone, and 800 parts of water;
[0066] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0067] Comparative Example 1
[0068] A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 30 parts of ferric tartrate, 10 parts of pyridine, 5 parts of 3-butene-1-amine, 20 parts of hydroquinone, and 500 parts of water;
[0069] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0070] Comparative Example 2
[0071] A high-efficiency complex iron desulfurizer comprises the following components in parts by weight: 30 parts of ferric ethylenediaminetetraacetate, 10 parts of pyridine, 5 parts of 3-butene-1-amine, 20 parts of hydroquinone, and 500 parts of water;
[0072] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0073] Comparative Example 3
[0074] A high-efficiency complex iron desulfurizer, comprising the following components in parts by weight: 25 parts of ferric citrate, 5 parts of ferric ethylenediaminetetraacetate, 10 parts of pyridine, 5 parts of 3-butene-1-amine, 20 parts of hydroquinone, and 500 parts of water;
[0075] The preparation method comprises the following steps: uniformly mixing the components to obtain a desulfurizing agent.
[0076] Experimental example
[0077] 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. After that, the gas is separated from the water by the demister at the top of the desulfurization tower. The gas after the droplets are separated is discharged from the top outlet of the desulfurization tower and enters the next gas-using section.
[0078] 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. The specific operating parameters were controlled as follows:
[0079] 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;
[0080] Calculation of desulfurization efficiency (K): K = (C1-C2) / C1×100%; the result is rounded to four decimal places, where C1 and C2 represent the volume fractions of hydrogen sulfide in the inlet and outlet gases, respectively. The outlet gas hydrogen sulfide volume fraction C2 is tested using GB / T 11060.11-2014 "Determination of sulfur compounds in natural gas - Part 11: Determination of hydrogen sulfide content by the coloring length detection tube method." The test results are shown in Table 1 below.
[0081] Table 1 Desulfurization test results
[0082]
[0083] Compared with Comparative Examples 1 to 3, the desulfurization efficiency of Example 1 is significantly improved, indicating that ferric tartrate can produce synergy with ethylenediaminetetraacetic acid iron, and can significantly improve desulfurization efficiency. Compared with Examples 2 and 4, the desulfurization efficiency of Examples 5 to 7 is significantly improved, indicating that when ferric tartrate and ethylenediaminetetraacetic acid iron ratio are 3 to 5: 1, desulfurization efficiency can be further improved. The desulfurization efficiency of Example 6 is greater than that of Example 5 and 7, which indicates that when ferric tartrate and ethylenediaminetetraacetic acid iron ratio are 4: 1, 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 synergy with diallylamine, and can further improve desulfurization efficiency. The desulfurization efficiency of Examples 12 to 14 is greater than that of Examples 10 to 11, indicating that when 3-butene-1-amine and diallylamine ratio are 1 to 3: 1, 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.
[0084] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.
Claims
1. A high-efficiency 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 ferric ethylenediaminetetraacetate, 10-20 parts of absorbent, 5-20 parts of stabilizer, 20-30 parts of synergist, and 500-1000 parts of water; The stabilizer is 3-butene-1-amine and diallylamine, and the weight ratio of the 3-butene-1-amine to diallylamine is 1-3:
1.
2. A high-efficiency 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 high-efficiency 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 high-efficiency complex iron desulfurizer according to claim 1, characterized in that: The absorbent includes one or both of pyridine and pyrrole.
5. A high-efficiency complex iron desulfurizer according to claim 1, characterized in that: The weight ratio of the 3-butene-1-amine to diallylamine is 2:
1.
6. A high-efficiency complex iron desulfurizer according to claim 1, characterized in that: The synergist includes one or more of hydroquinone, piperazine, and sulfolane.
7. The method for preparing a high-efficiency complex iron desulfurizer according to any one of claims 1 to 6, characterized in that: The following steps are involved: The components are mixed uniformly to obtain the desulfurizing agent.
8. Use of the high-efficiency complex iron desulfurizer according to any one of claims 1 to 6 or the desulfurizer prepared by the preparation method according to claim 7 in the field of desulfurization technology.
Citation Information
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Liquid absorbent for removing hydrogen sulfide and application thereof
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