CN116059812A - Synthesis method of complex iron ion desulfurizing agent - Google Patents

Synthesis method of complex iron ion desulfurizing agent Download PDF

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CN116059812A
CN116059812A CN202211567277.3A CN202211567277A CN116059812A CN 116059812 A CN116059812 A CN 116059812A CN 202211567277 A CN202211567277 A CN 202211567277A CN 116059812 A CN116059812 A CN 116059812A
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iron ion
solution
desulfurizer
molar ratio
iron
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黎文亮
郭柏序
曹焕尧
杨开帅
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CHENGDU HUAYANGXINGHUA CHEMICAL
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/48—Sulfur compounds
    • B01D53/52—Hydrogen sulfide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/77—Liquid phase processes
    • B01D53/78—Liquid phase processes with gas-liquid contact
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
    • C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
    • C10L3/10—Working-up natural gas or synthetic natural gas
    • C10L3/101—Removal of contaminants
    • C10L3/102—Removal of contaminants of acid contaminants
    • C10L3/103—Sulfur containing contaminants

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Abstract

The invention belongs to the technical field of hydrogen sulfide-containing gas purification, and in particular relates to a synthesis method of a complex iron ion desulfurizer, which comprises the steps of mixing nitrilotriacetic acid and ethylenediamine tetraacetic acid according to a molar ratio of 1:1-1:2, mixing ferric oxide and the mixture according to a molar ratio of 1:1-1:2, adding water as a solvent, heating the mixed solution to 95-100 ℃, gradually adding an accelerator into the mixed solution, stirring the solution, and ending the reaction after all solids in the solution are dissolved.

Description

一种络合铁离子脱硫剂的合成方法A kind of synthetic method of complex iron ion desulfurizer

技术领域technical field

本发明属于含硫化氢气体净化技术领域，具体涉及一种络合铁离子脱硫剂的合成方法。The invention belongs to the technical field of hydrogen sulfide-containing gas purification, and in particular relates to a synthesis method of a complex iron ion desulfurizer.

背景技术Background technique

湿式氧化还原法络合铁脱硫技术采用三价铁离子将天然气中硫化氢直接转化成单质硫，三价铁离子被还原成二价铁离子，二价铁离子可采用空气进行再生，通过空气中的氧气氧化成三价铁离子，是一种工艺简单、工作硫容高且环保无毒的新型脱硫技术，克服了传统脱硫工艺硫容量低、脱硫工艺复杂、副盐生成率高、环境污染严重等弊端。目前常规的铁离子脱硫剂铁离子采用螯合剂与氯化铁或硫酸铁铵进行复配，这种方法合成的铁离子螯合力弱，容易损耗，有效含量低，因此，硫容较低。Wet oxidation-reduction complex iron desulfurization technology uses ferric ions to directly convert hydrogen sulfide in natural gas into elemental sulfur, and the ferric ions are reduced to ferrous ions, which can be regenerated by air. Oxygen is oxidized into ferric ions, which is a new type of desulfurization technology with simple process, high working sulfur capacity, and environmental protection and non-toxicity. and other disadvantages. At present, the conventional iron ion desulfurizer iron ion is compounded with chelating agent and ferric chloride or ferric ammonium sulfate. The iron ion synthesized by this method has weak chelating ability, is easy to be lost, and has low effective content. Therefore, the sulfur capacity is low.

发明内容Contents of the invention

本发明针对现有技术的不足，目的在于提供一种稳定性好，含量高的络合铁离子脱硫剂。The invention aims at the deficiencies of the prior art and aims to provide a complex iron ion desulfurizer with good stability and high content.

为实现上述发明目的，本发明采用的技术方案为：For realizing above-mentioned purpose of the invention, the technical scheme that the present invention adopts is:

一种络合铁离子脱硫剂的合成方法，包括以下步骤：将次氮基三乙酸和乙二胺四乙酸按摩尔比1:1～1:2混合，再将氧化铁与上述混合物按摩尔比1:1～1：2混合，加入水作为溶剂，将混合液加热至95-100℃，逐步向混合液中添加促进剂，同时对溶液进行搅拌，待溶液中固体全部溶解后即反应结束，形成络合铁离子脱硫剂。A method for synthesizing a complex iron ion desulfurizer, comprising the following steps: mixing nitrilotriacetic acid and ethylenediaminetetraacetic acid in a molar ratio of 1:1 to 1:2, and then mixing iron oxide with the above-mentioned mixture in a molar ratio Mix 1:1～1:2, add water as a solvent, heat the mixture to 95-100°C, gradually add accelerators to the mixture, and stir the solution at the same time, and the reaction ends after all the solids in the solution are dissolved. Form complex iron ion desulfurizer.

上述方案中，所述氧化铁为Fe2O3·H2O或Fe2O3。In the above solution, the iron oxide is Fe 2 O 3 ·H 2 O or Fe 2 O 3 .

上述方案中，所述促进剂包括碳酸钠与氨水的混合物，所述碳酸钠与氨水摩尔比为1:2，搅拌速率为60～120转/分钟。In the above scheme, the accelerator includes a mixture of sodium carbonate and ammonia water, the molar ratio of sodium carbonate and ammonia water is 1:2, and the stirring speed is 60-120 rpm.

本发明的有益效果如下：The beneficial effects of the present invention are as follows:

常规络合铁离子脱硫剂利用螯合剂与氯化铁或硫酸铁铵进行复配，生产的螯合铁不能完全与铁形成稳定的螯合共价键结构，使得铁离子在碱性溶液中容易与OH-或CO3 2-反应，生成氢氧化铁或者碳酸铁沉淀，从而造成铁离子的损失。本发明针对以上问题，采用氧化铁与氮基三乙酸、乙二胺四乙酸化学反应合成的方法生成次氮基三乙酸铁和乙二胺四乙酸铁，这种螯合铁离子为空间立体结构，能够通过立体共价键使铁离子在碱性溶液中稳定以离子形态存在，避免生成氢氧化铁或者碳酸铁沉淀，大幅度降低铁离子损耗，从而使脱硫剂含量更高、硫容更大，脱硫效率更高。Conventional chelated iron ion desulfurizers use chelating agents to compound ferric chloride or ferric ammonium sulfate, and the produced chelated iron cannot completely form a stable chelated covalent bond structure with iron, making it easy for iron ions to interact with iron in alkaline solutions. OH - or CO 3 2- react to generate iron hydroxide or iron carbonate precipitation, resulting in the loss of iron ions. The present invention aims at the above problems, and adopts the method for chemical reaction synthesis of iron oxide, nitrilotriacetic acid and ethylenediaminetetraacetic acid to generate iron nitrilotriacetate and iron ethylenediaminetetraacetic acid, and this chelated iron ion is a three-dimensional structure , can stabilize iron ions in alkaline solution in the form of ions through stereocovalent bonds, avoid the formation of iron hydroxide or iron carbonate precipitation, and greatly reduce the loss of iron ions, so that the content of desulfurizer is higher and the sulfur capacity is larger , the desulfurization efficiency is higher.

具体实施方式Detailed ways

为了更好地理解本发明，下面结合实施例进一步阐明本发明的内容，但本发明的内容不仅仅局限于下面的实施例。In order to better understand the present invention, the content of the present invention is further illustrated below in conjunction with the examples, but the content of the present invention is not limited to the following examples.

实施例1传统脱硫剂的制备The preparation of embodiment 1 traditional desulfurizer

将硫酸铁铵、乙二胺四乙酸配制成水溶液，配制浓度如下表。脱硫剂中铁离子浓度10g/L,加入NaOH调解溶液pH值8-9,配制方式如下表。Prepare ferric ammonium sulfate and ethylenediaminetetraacetic acid into an aqueous solution, and the prepared concentration is as shown in the table below. The iron ion concentration in the desulfurizer is 10g/L, and NaOH is added to adjust the pH value of the solution to 8-9. The preparation method is as follows.

脱硫剂组成如下表所示：The composition of the desulfurizer is shown in the table below:

组分components 用量Dosage 硫酸铁铵ammonium ferric sulfate 47.5g47.5g 水water 900g900g 乙二胺四乙酸Ethylenediaminetetraacetic acid 100g100g NaOHNaOH 5g5g

将含有1000ppm硫化氢的氮气混合物通入上述脱硫剂溶液中，待出口硫化氢含量超过10pppm停止通气，然后向溶液中通入30分钟空气(1L/min)后，重复以上步骤共计3个循环，检测铁离子浓度如下为7.5g/L，铁离子损失率为(10-7.5)/10×100％＝25％。Pass the nitrogen mixture containing 1000ppm hydrogen sulfide into the above-mentioned desulfurizer solution, stop the ventilation when the outlet hydrogen sulfide content exceeds 10ppm, then pass air (1L/min) into the solution for 30 minutes, repeat the above steps for a total of 3 cycles, The detected iron ion concentration is 7.5 g/L as follows, and the iron ion loss rate is (10-7.5)/10×100%=25%.

实施例2本发明脱硫剂的制备Embodiment 2 Preparation of desulfurizer of the present invention

将氧化铁、次氮基三乙酸、乙二胺四乙酸混合，加入水加热至95℃，搅拌转速60转/分钟，2小时内匀速加入碳酸钠、氨水(摩尔比1:2)的促进剂，生产络合铁离子脱硫剂。配制浓度如下表。脱硫剂中铁离子浓度10g/L,加入NaOH调解溶液pH值8～9,配制方式如下表。Mix iron oxide, nitrilotriacetic acid, and ethylenediaminetetraacetic acid, add water, heat to 95°C, stir at 60 rpm, and add sodium carbonate and ammonia water (molar ratio 1:2) at a uniform speed within 2 hours. , Production of complex iron ion desulfurizer. The preparation concentration is shown in the table below. The iron ion concentration in the desulfurizer is 10g/L, and NaOH is added to adjust the pH value of the solution to 8-9. The preparation method is as follows.

脱硫剂组成如下表所示：The composition of the desulfurizer is shown in the table below:

组分components 用量Dosage 氧化铁iron oxide 14.29g14.29g 次氮基三乙酸nitrilotriacetic acid 17.05g17.05g 乙二胺四乙酸Ethylenediaminetetraacetic acid 26.07g26.07g 碳酸钠、氨水混合物(摩尔比1:2)Sodium carbonate, ammonia water mixture (molar ratio 1:2) 45g45g 水water 945g945g NaOHNaOH 5g5g

将含有1000ppm硫化氢的氮气混合物通入上述脱硫剂溶液中，待出口硫化氢含量超过10pppm停止通气，然后向溶液中通入30分钟空气(1L/min)后，重复以上步骤共计3个循环，检测铁离子浓度如下为9.95g/L，铁离子损失率为(10-9.95)/10×100％＝0.5％。Pass the nitrogen mixture containing 1000ppm hydrogen sulfide into the above-mentioned desulfurizer solution, stop the ventilation when the outlet hydrogen sulfide content exceeds 10ppm, then pass air (1L/min) into the solution for 30 minutes, repeat the above steps for a total of 3 cycles, The detected iron ion concentration is 9.95g/L as follows, and the iron ion loss rate is (10-9.95)/10×100%=0.5%.

实施例3本发明脱硫剂的制备Embodiment 3 Preparation of desulfurizing agent of the present invention

将氧化铁、次氮基三乙酸、乙二胺四乙酸混合，加入水加热至98℃，搅拌转速100转/分钟，2.5小时内匀速加入碳酸钠、氨水(摩尔比1:2)的促进剂，生产络合铁离子脱硫剂。配制浓度如下表。脱硫剂中铁离子浓度10g/L,加入NaOH调解溶液pH值8～9,配制方式如下表。Mix iron oxide, nitrilotriacetic acid, and ethylenediaminetetraacetic acid, add water, heat to 98°C, stir at 100 rpm, and add sodium carbonate and ammonia water (molar ratio 1:2) at a uniform speed within 2.5 hours. , Production of complex iron ion desulfurizer. The preparation concentration is shown in the table below. The iron ion concentration in the desulfurizer is 10g/L, and NaOH is added to adjust the pH value of the solution to 8-9. The preparation method is as follows.

脱硫剂组成如下表所示：The composition of the desulfurizer is shown in the table below:

Figure BDA0003986591350000031
Figure BDA0003986591350000031

Figure BDA0003986591350000041
Figure BDA0003986591350000041

将含有1000ppm硫化氢的氮气混合物通入上述脱硫剂溶液中，待出口硫化氢含量超过10pppm停止通气，然后向溶液中通入30分钟空气(1L/min)后，重复以上步骤共计3个循环，检测铁离子浓度如下为9.93g/L，铁离子损失率为(10-9.93)/10×100％＝0.7％。Pass the nitrogen mixture containing 1000ppm hydrogen sulfide into the above-mentioned desulfurizer solution, stop the ventilation when the outlet hydrogen sulfide content exceeds 10ppm, then pass air (1L/min) into the solution for 30 minutes, repeat the above steps for a total of 3 cycles, The detected iron ion concentration is 9.93g/L as follows, and the iron ion loss rate is (10-9.93)/10×100%=0.7%.

实施例4本发明脱硫剂的制备Embodiment 4 Preparation of desulfurizing agent of the present invention

本发明络合铁离子实施例。将氧化铁、次氮基三乙酸、乙二胺四乙酸混合，加入水加热至100℃，搅拌转速120转/分钟，3小时内匀速加入碳酸钠、氨水(摩尔比1:2)的促进剂，生产络合铁离子脱硫剂。配制浓度如下表。脱硫剂中铁离子浓度10g/L,加入NaOH调解溶液pH值8～9,配制方式如下表。The present invention is an embodiment of complexed iron ions. Mix iron oxide, nitrilotriacetic acid, and ethylenediaminetetraacetic acid, add water and heat to 100°C, stir at a speed of 120 rpm, and add sodium carbonate and ammonia water (molar ratio 1:2) at a uniform speed within 3 hours. , Production of complex iron ion desulfurizer. The preparation concentration is shown in the table below. The iron ion concentration in the desulfurizer is 10g/L, and NaOH is added to adjust the pH value of the solution to 8-9. The preparation method is as follows.

脱硫剂组成如下表所示：The composition of the desulfurizer is shown in the table below:

组分components 用量Dosage 氧化铁iron oxide 14.29g14.29g 次氮基三乙酸nitrilotriacetic acid 8.52g8.52g 乙二胺四乙酸Ethylenediaminetetraacetic acid 13.03g13.03g 碳酸钠、氨水混合物(摩尔比1:2)Sodium carbonate, ammonia water mixture (molar ratio 1:2) 45g45g 水water 966g966g NaOHNaOH 5g5g

将含有1000ppm硫化氢的氮气混合物通入上述脱硫剂溶液中，待出口硫化氢含量超过10pppm停止通气，然后向溶液中通入30分钟空气(1L/min)后，重复以上步骤共计3个循环，检测铁离子浓度如下为9.91g/L，铁离子损失率为(10-9.93)/10×100％＝0.9％。Pass the nitrogen mixture containing 1000ppm hydrogen sulfide into the above-mentioned desulfurizer solution, stop the ventilation when the outlet hydrogen sulfide content exceeds 10ppm, then pass air (1L/min) into the solution for 30 minutes, repeat the above steps for a total of 3 cycles, The detected iron ion concentration is 9.91 g/L as follows, and the iron ion loss rate is (10-9.93)/10×100%=0.9%.

通过以上实施例发现，本发明络合铁离子脱硫剂损耗量比传统铁离子脱硫剂损耗量大幅度降低，从而降低生产消耗，提高产品质量。Through the above examples, it is found that the loss of the complex iron ion desulfurizer of the present invention is significantly lower than that of the traditional iron ion desulfurizer, thereby reducing production consumption and improving product quality.

Claims (3)

1. The synthesis method of the complex iron ion desulfurizing agent is characterized by comprising the following steps of: mixing nitrilotriacetic acid and ethylenediamine tetraacetic acid according to a molar ratio of 1:1-1:2, and mixing ferric oxide and the mixture according to a molar ratio of 1:1-1: 2 mixing, adding water as solvent, heating the mixed solution to 95-100 ℃, gradually adding accelerator into the mixed solution, stirring the solution, and finishing the reaction after all solids in the solution are dissolved.
2. The method according to claim 1, wherein the iron oxide is Fe 2 O 3 ·H 2 O or Fe 2 O 3 。
3. The method of claim 1, wherein the accelerator comprises a mixture of sodium carbonate and aqueous ammonia, the molar ratio of sodium carbonate to aqueous ammonia is 1:2, and the stirring rate is 60-120 rpm.
CN202211567277.3A 2022-12-07 2022-12-07 Synthesis method of complex iron ion desulfurizing agent Pending CN116059812A (en)

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CN116422382A (en) * 2023-06-13 2023-07-14 山东秋水化学科技有限公司 Wet desulfurization complex iron catalyst and preparation method thereof
CN117654640A (en) * 2024-02-01 2024-03-08 成都华阳兴华化工有限公司 Iron ion catalytic desulfurizing agent and preparation method and application thereof

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CN1135183A (en) * 1994-12-27 1996-11-06 明纳托产业株式会社 Deodorizing composition and deodorizing resin composition both contg. iron 2 compound
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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN116422382A (en) * 2023-06-13 2023-07-14 山东秋水化学科技有限公司 Wet desulfurization complex iron catalyst and preparation method thereof
CN117654640A (en) * 2024-02-01 2024-03-08 成都华阳兴华化工有限公司 Iron ion catalytic desulfurizing agent and preparation method and application thereof

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