CN102703149A - Method for natural gas desulphurization and resource utilization of desulphurization waste solution - Google Patents
Method for natural gas desulphurization and resource utilization of desulphurization waste solution Download PDFInfo
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- CN102703149A CN102703149A CN2012101649994A CN201210164999A CN102703149A CN 102703149 A CN102703149 A CN 102703149A CN 2012101649994 A CN2012101649994 A CN 2012101649994A CN 201210164999 A CN201210164999 A CN 201210164999A CN 102703149 A CN102703149 A CN 102703149A
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Abstract
The invention provides a method for natural gas desulphurization and resource utilization of desulphurization waste solution. The method comprises the following steps: determining liquid sodium hydroxide or sodium carbonate as absorption liquid for natural gas to absorb H2S and CO2 in the natural gas, ensuring that the absorption reaction reaches an end point by adjusting the pH value, converting the absorption liquid into absorption liquid of a sodium sulfhydrate or sodium bicarbonate system, adding sodium hydroxide solution, further converting the absorption liquid into the absorption liquid of the sodium sulfide and sodium carbonate system, then adding liquid barium sulfide, and extracting industrial products barium carbonate and sodium sulfide after reaction. The method is totally different from the conventional desulphurization technology, realizes clean production without three-waste pollutant discharged in the whole technological process, simply and thoroughly solves the problem that the existing natural gas desulphurization method pollutes the environment, and simultaneously improves the labor productivity, reduces the energy consumption, and has high added value in obtained resource products, simple process flow and obvious environmental and economic benefits.
Description
Technical field
The present invention relates to the natural gas conditioning technology, particularly selexol process, decarburization, and the waste liquid that produces clean treatment process, be specifically related to
OnePlant the method for selexol process and desulfurization waste liquor recycling.
Background technology
Sweet natural gas be clean the most, efficiently, the incendivity energy easily.Rationally utilize Sweet natural gas, abundant purified natural gas, can optimize energy consumption structure, improve atmospheric environment, realize target for energy-saving and emission-reduction, society is significant to the friendly type of built environment.Sweet natural gas comprises and do not contain or contain trace sulfide and carbonic acid gas, and need not purifying treatment can beyond defeated and the direct clean gas of utilization; Also comprising gases such as the sulfide that contains significant quantity and carbonic acid gas, is the sour natural gas that must after purifying treatment, just can reach defeated standard of pipe or commodity gas gas quality index.The sulfide that exists in latter's Sweet natural gas is mainly hydrogen sulfide, contains some organic sulfides in addition, as: toxic and harmfuls such as mercaptan, thioether, COS and dithiocarbonic anhydride.Visible from the contained material composition of sour natural gas, its sulfur component mainly is a hydrogen sulfide, for severe toxicity and distribute unpleasant stink, contaminate environment, be detrimental to health, and metal is had corrosive nature; If the too high meeting of carbon dioxide content reduces the calorific value of Sweet natural gas.Therefore, must carry out desulfurization and decarburization to sour natural gas and handle, particularly desulfurization is handled, and could use.At present, the chemical absorption method that the selexol process treatment process that discloses is both at home and abroad worked as with wet desulphurization is main.Chemical absorption method is to absorb most acidic components in the natural gas through lyosorption, and remaining acidic components remake absorption extraction further, must finally reach the requirement of commodity gas gas quality index through long technical process.In the said process, because the H that desorption tower was rich in
2The S acid gas is a kind of have stench, big hypertoxic gas of amount, therefore must be with H
2The S processing treatment becomes sulfur product to reclaim.Traditional treatment process is to adopt Kraus process to be prepared into sulphur.But because Kraus process investment is big, output is low, running cost is high, some middle-size and small-size oil gas factories are hung back, be difficult to bear this with high cost with H
2S is prepared into the method for sulphur.For many years, the sour gas of small-sized oil gas factory is to adopt directly discharging behind the torch burning basically, is difficult to effect a radical cure pollution problem.Therefore, how resolving the desulphurization problem of Sweet natural gas, is urgent problem in the industry.
Summary of the invention
The present invention proposes the method for the recycling of a kind of selexol process and desulfurization waste liquor; Purpose is to abandon traditional Kraus process; But ward off new footpath in addition; Thoroughly solve selexol process and handle the problem of environmental pollution that is brought, and fully reclaim available stock wherein, to realize the remarkable lifting of environmental benefit and economic benefit.
Technical solution of the present invention:
One, technological line of the present invention: confirm that liquid hydrogen sodium oxide or yellow soda ash are the absorption liquid of Sweet natural gas, with the H of this absorption liquid in absorption tower internal adsorption weather is right
2S and CO
2, adjustment pH value is reached home absorption reaction, and is converted into Sodium sulfhydrate and sodium hydrogencarbonate system absorption liquid; Add sodium hydroxide solution again, Sodium sulfhydrate and sodium hydrogencarbonate system absorption liquid are converted into sodium sulphite and yellow soda ash system absorption liquid; Add barium sulfide solution again, react at a certain temperature, extract industrial goods barium carbonate and industrial goods sodium sulphite at last.
Two, definite foundation of technological line of the present invention:
(1) confirming that liquid hydrogen sodium oxide or yellow soda ash are the absorption liquid of Sweet natural gas, is according to the following principles of chemistry:
Sodium hydroxide and H
2The S reaction generates Sodium sulfhydrate and water: NaOH+H
2S===NaHS+H
2O;
Sodium hydroxide and CO
2Reaction generates sodium hydrogencarbonate: NaOH+CO
2The NaHCO of===
3
Yellow soda ash and H
2The S reaction generates Sodium sulfhydrate and sodium hydrogencarbonate
Na
2CO
3+?H
2S?===?NaHS+NaHCO
3
Yellow soda ash and CO
2Reaction generates sodium hydrogencarbonate:
Na
2CO
3+CO
2+H
2O?===?2NaHCO
3
Above-mentioned reaction terminating, the solute of absorption liquid changes, and changes Sodium sulfhydrate and sodium hydrogencarbonate system into.
(2) with absorption liquid Sodium sulfhydrate and sodium hydrogencarbonate system, add sodium hydroxide solution, be converted into sodium sulphite and yellow soda ash system, institute according to the principles of chemistry is:
Sodium sulfhydrate and sodium hydroxide reaction generate sodium sulphite and water:
NaHS+NaOH===?Na
2S+H
2O
Sodium hydrogencarbonate and sodium hydroxide reaction generate yellow soda ash and water:
NaHCO
3+ NaOH===Na
2CO
3+ H
2The above-mentioned reaction terminating of O, the solute of absorption liquid changes, and changes sodium sulphite and yellow soda ash system into.
(3) absorption liquid with sodium sulphite and yellow soda ash system adds liquid curing barium, generates precipitated barium carbonate and sodium sulphite, and institute according to the principles of chemistry is: wherein, and yellow soda ash and barium sulphide reaction, Na
2CO
3+ BaS===BaCO
3↓+Na
2S
The generation precipitated barium carbonate is separated out, and mother liquor is the aqueous solution of sodium sulphite.Handle through routine again and obtain industrial goods vulcanized sodium and industrial goods brium carbonate.
Three, process step of the present invention is following:
(1) a: the preparation quality percentage concentration is that the sodium hydroxide absorption liquid of 3-5% is subsequent use; Or the preparation quality percentage concentration is that the yellow soda ash absorption liquid of 5-8% is subsequent use; (in sweetening process, fibrous root is the border situation factually, selects one of which to use according to qualifications)
B: the mass percent concentration of preparation sodium hydroxide reaction solution is that 8-10% is subsequent use;
C: the mass percent concentration of formulating vulcanization barium reaction solution is that 10-15% is subsequent use;
(2) sodium hydroxide absorption liquid that step () a is subsequent use or subsequent use yellow soda ash absorption liquid are inserted in the absorption tower; Feed pending Sweet natural gas, the pH value of control absorption liquid is when pH=11-12; Absorption reaction is reached home; The solute of absorption liquid is Sodium sulfhydrate or sodium hydrogencarbonate system, from the absorption tower, shifts out reaction solution simultaneously, carries out next process step again.
(3) sodium hydroxide solution that step () b is subsequent use add step (two) Sodium sulfhydrate or with sodium hydrogencarbonate absorption liquid system in; The pH value of control response behaviour absorption liquid; When pH=14, reaction is reached home, and the solute of absorption liquid is sodium sulphite and yellow soda ash system.
(4) the subsequent use barium sulfide solution of step () c is joined in the absorption liquid of sodium sulphite and yellow soda ash system, temperature of reaction is controlled at 80-90 ℃, separates out the barium carbonate white precipitate, when deposition no longer continues, is reaction end;
(5) absorption liquid of step (four) is made solid-liquid separation and extract barium carbonate; And to barium carbonate wash, suction filtration, drying, make the industrial goods barium carbonate;
(6) with the aqueous solution of the Containing Sulfur sodium after step (five) solid-liquid separation, evaporate, concentrate, collect water of condensation simultaneously, when the mass percent concentration of liquid concentrator is 60%, stop to concentrate, obtain industrial goods sodium sulphite; Collected water of condensation recycling is used for the absorption liquid of obtaining liq sodium hydroxide or yellow soda ash.
Beneficial effect of the present invention:
(1) the present invention is different from the desulfurization technology of traditional Crouse's method fully; But adopt liquid sodium hydroxide or liquid carbonic acid sodium is natural gas desulfurization absorption liquid, and the waste liquid after the desulfurization need not regeneration, and has obtained recycling treatment; Eliminate backward production facilities, improved labour productivity; And reduced consumption to the energy, have remarkable social benefit.
(2) the present invention has also made full use of the effective constituent in the desulfurization waste liquor; Through adding the part industrial chemicals; Accomplished non-pollutant discharge; Solved the pollution problem that existing natural gas desulfur method brings to environment simply, up hill and dale, whole technological process belongs to the production that cleans of not having " three wastes " generation, and has significant environmental benefit.
(3) the inventive method is compared with existing natural gas desulfur method, and the added value of the resource product that obtains is high, and technical process is simple, has remarkable economic efficiency.
Description of drawings
Accompanying drawing 1 is the inventive method main technique FB(flow block).
Embodiment
It is as shown in the figure,
The main technique flow process of the inventive method is the preparation of sodium hydroxide or yellow soda ash absorption liquid; Absorption liquid absorbs H
2S and CO
2, adjustment pH value=11-12 gets the mixed liquid of Sodium sulfhydrate and sodium hydrogencarbonate; Add sodium hydroxide solution again, adjustment pH value=14 get the mixed liquid of sodium sulphite and yellow soda ash; Add barium sulfide solution again, under the certain temperature condition, absorption reaction is reached home, and be converted into the absorption liquid of sodium sulphite and barium carbonate system, through suction filtration, solid is the industrial goods barium carbonate; Liquid is the sodium sulphite mother liquor, through concentrate industrial goods sodium sulphite; Collected water of condensation recycling is used to prepare sodium hydroxide or yellow soda ash absorption liquid.
Below provide embodiment:
Embodiment one:
1, preparation sodium hydroxide absorption liquid, volume is 1 liter; Mass percent concentration is 5%;
2, preparation sodium hydroxide solution, volume is 1 liter; Mass percent concentration is 10%;
3, preparation barium sulfide solution, volume is 1 liter; Mass percent concentration is 15%;
4, with 1 liter of sodium hydroxide absorption liquid and H
2The content of S is 1%,, CO
2Content be that 4.5% Sweet natural gas carries out gas liquid reaction for 1000 liters, when recording the pH=12 of absorption liquid, stopped reaction; 0.5 liter of the sodium hydroxide solution that adds above-mentioned 10% concentration in the absorption liquid records the pH=14 of absorption liquid; When heating absorption liquid to 80 ℃ then, add 1 liter of the barium sulfide solution of above-mentioned 15% concentration, separate out white precipitate in the reaction; Carry out solid-liquid separation; Washing, suction filtration, oven dry white precipitate then obtain Powdered industrial potassium titanate 200 grams; With the mother liquor after separating concentrate, when the mass percent of liquid concentrator is 60%, stop to concentrate, the quality of gained enriched material is 170 grams, is content and is 60% industrial goods sodium sulphite.
Embodiment two:
1, preparation yellow soda ash absorption liquid, volume is 2 liters; Mass percent concentration is 8%;
2, preparation sodium hydroxide solution, volume is 1 liter; Mass percent concentration is 10%;
3, preparation barium sulfide solution, volume is 3 liters; Mass percent concentration is 15%;
4, with 1.6 liters of sodium hydroxide absorption liquids and H
2The content of S is 1%,, CO
2Content be that 4.5% Sweet natural gas carries out gas liquid reaction for 1000 liters, when recording the pH=12 of absorption liquid, stopped reaction; 1 liter of the sodium hydroxide solution that adds above-mentioned 10% concentration in the absorption liquid records the pH=14 of absorption liquid; When heating absorption liquid to 80 ℃ then, add 2.2 liters of the barium sulfide solutions of above-mentioned 15% concentration, separate out white precipitate in the reaction; Carry out solid-liquid separation; Washing, suction filtration, oven dry white precipitate then obtain Powdered industrial potassium titanate 460 grams; With the mother liquor after separating concentrate, when the mass percent of liquid concentrator is 60%, stop to concentrate, the quality of gained enriched material is 340 grams, is content and is 60% industrial goods sodium sulphite.
Embodiment three:
1, preparation sodium hydroxide absorption liquid, volume is 2 liters; Mass percent concentration is 3%;
2, preparation sodium hydroxide solution, volume is 0.5 liter; Mass percent concentration is 8%;
3, preparation barium sulfide solution, volume is 1 liter; Mass percent concentration is 10%;
4, with 1.45 liters of sodium hydroxide absorption liquids and H
2The content of S is 1.5%,, CO
2Content be that 3% Sweet natural gas carries out gas liquid reaction for 1000 liters, when recording the pH=11 of absorption liquid, stopped reaction; 0.5 liter of the sodium hydroxide solution that adds above-mentioned 8% concentration in the absorption liquid records the pH=14 of absorption liquid; When heating absorption liquid to 75 ℃ then, the barium sulphide that adds above-mentioned 10% concentration dissolves 1 liter, separates out white precipitate in the reaction; Carry out solid-liquid separation; Washing, suction filtration, oven dry white precipitate then obtain Powdered industrial potassium titanate 134 grams; With the mother liquor after separating concentrate, when the mass percent of liquid concentrator is 60%, stop to concentrate, the quality of gained enriched material is 145 grams, is content and is 60% industrial goods sodium sulphite.
Embodiment four:
1, preparation yellow soda ash absorption liquid, volume is 2.3 liters; Mass percent concentration is 5%;
2, preparation sodium hydroxide solution, volume is 1 liter; Mass percent concentration is 8%;
3, preparation barium sulfide solution, volume is 3 liters; Mass percent concentration is 10%;
4, with 2.3 liters of yellow soda ash absorption liquids and H
2The content of S is 1.5%,, CO
2Content be that 3% Sweet natural gas carries out gas liquid reaction for 1000 liters, when recording the pH=12 of absorption liquid, stopped reaction; 1 liter of the sodium hydroxide solution that adds above-mentioned 8% concentration in the absorption liquid records the pH=14 of absorption liquid; When heating absorption liquid to 70 ℃ then, add 3 liters of the barium sulfide solutions of above-mentioned concentration, separate out white precipitate in the reaction; Carry out solid-liquid separation; Washing, suction filtration, oven dry white precipitate then obtain Powdered industrial potassium titanate 354 grams; With the mother liquor after separating concentrate, when the mass percent of liquid concentrator is 60%, stop to concentrate, the quality of gained enriched material is 290 grams, is content and is 60% industrial goods sodium sulphite.
To sum up; The present invention compares with the method for the right desulfurization of existing weather, has fundamentally solved the pollution problem of technological process to environment, and the technical grade product purity that is obtained is high, added value is high; Production technique is simple, process cleans, non-pollutant discharge, has really reached the goal of the invention of expection.
Claims (3)
1. the method for the recycling of selexol process and desulfurization waste liquor, it is characterized in that: the technological line of present method is to confirm that liquid hydrogen sodium oxide or yellow soda ash are the absorption liquid of Sweet natural gas, with the H in this absorption liquid absorption natural gas
2S and CO
2, adjustment pH value is reached home absorption reaction, is converted into Sodium sulfhydrate and sodium hydrogencarbonate system absorption liquid; Add sodium hydroxide solution again, Sodium sulfhydrate and sodium hydrogencarbonate system absorption liquid are converted into sodium sulphite and yellow soda ash system absorption liquid; Add barium sulfide solution again and react, extract industrial goods barium carbonate and industrial goods sodium sulphite at last.
2. the method for the recycling of a kind of selexol process according to claim 1 and desulfurization waste liquor is characterized in that: the process step of said technological line is following:
(1) a: the preparation quality percentage concentration is that the sodium hydroxide absorption liquid of 3-5% is subsequent use; Or the preparation quality percentage concentration is that the yellow soda ash absorption liquid of 5-8% is subsequent use;
B: the mass percent concentration of preparation sodium hydroxide reaction solution is that 8-10% is subsequent use;
C: the mass percent concentration of formulating vulcanization barium reaction solution is that 10-15% is subsequent use;
(2) sodium hydroxide absorption liquid that step () a is subsequent use or subsequent use yellow soda ash absorption liquid are inserted in the absorption tower; Feed pending Sweet natural gas, the pH value of control absorption liquid is when pH=11-12; Absorption reaction is reached home, and the solute of absorption liquid is Sodium sulfhydrate and sodium hydrogencarbonate system;
(3) step () b is subsequent use sodium hydroxide solution adds in the Sodium sulfhydrate and sodium hydrogencarbonate absorption liquid system of step (two); The pH value of control response behaviour absorption liquid; When pH=14, reaction is reached home, and the solute of absorption liquid is sodium sulphite and yellow soda ash system;
(4) the subsequent use barium sulfide solution of step () c is joined in the absorption liquid of sodium sulphite and yellow soda ash system, temperature of reaction is controlled at 80-90 ℃, separates out the barium carbonate white precipitate, when deposition no longer continues, is reaction end;
(5) absorption liquid of step (four) is made solid-liquid separation and extract barium carbonate; And to barium carbonate wash, suction filtration, drying, make the industrial goods barium carbonate;
(6) with the aqueous solution of the Containing Sulfur sodium after step (five) solid-liquid separation, evaporate, concentrate, collect water of condensation simultaneously, when the mass percent concentration of liquid concentrator is 60%, stop to concentrate, obtain industrial goods sodium sulphite.
3. the method for the recycling of a kind of selexol process according to claim 2 and desulfurization waste liquor is characterized in that: the water of condensation recycling of said collection is used to prepare the absorption liquid of sodium hydroxide or yellow soda ash.
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Cited By (7)
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| CN103693626A (en) * | 2013-12-18 | 2014-04-02 | 安徽工业大学 | Method for preparing sodium hydrosulfide from hydrogen sulfide acid gas containing carbon dioxide |
| CN103691282A (en) * | 2013-12-18 | 2014-04-02 | 安徽工业大学 | Method for preparing sodium carbonate from hydrogen sulfide acid gas |
| CN105731387A (en) * | 2014-12-06 | 2016-07-06 | 中国石油化工股份有限公司 | Method and apparatus for preparing sodium hydrosulfide by using acidic gas |
| CN106554835A (en) * | 2015-09-24 | 2017-04-05 | 中国石油化工股份有限公司 | A kind of removing of hydrogen sulfide in natural gas and recycling processing method |
| CN107746068A (en) * | 2017-10-17 | 2018-03-02 | 中国日用化学工业研究院 | A kind of silica modified barium sulfate raw powder's production technology |
| CN114854457A (en) * | 2022-01-20 | 2022-08-05 | 中国中煤能源集团有限公司 | Decarbonization and desulfurization method for mixed gas containing combustible gas |
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Cited By (11)
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| CN103611407A (en) * | 2013-12-18 | 2014-03-05 | 安徽工业大学 | Method for removing carbon dioxide from hydrogen sulfide acid gas by using buffer solution |
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| CN103691282B (en) * | 2013-12-18 | 2015-09-23 | 安徽工业大学 | A kind of method utilizing hydrogen sulfide acid gas to prepare sodium carbonate |
| CN105731387A (en) * | 2014-12-06 | 2016-07-06 | 中国石油化工股份有限公司 | Method and apparatus for preparing sodium hydrosulfide by using acidic gas |
| CN105731387B (en) * | 2014-12-06 | 2017-08-22 | 中国石油化工股份有限公司 | A kind of method and device that sodium acid carbonate is prepared by sour gas |
| CN106554835A (en) * | 2015-09-24 | 2017-04-05 | 中国石油化工股份有限公司 | A kind of removing of hydrogen sulfide in natural gas and recycling processing method |
| CN107746068A (en) * | 2017-10-17 | 2018-03-02 | 中国日用化学工业研究院 | A kind of silica modified barium sulfate raw powder's production technology |
| CN114854457A (en) * | 2022-01-20 | 2022-08-05 | 中国中煤能源集团有限公司 | Decarbonization and desulfurization method for mixed gas containing combustible gas |
| WO2023138706A1 (en) * | 2022-01-20 | 2023-07-27 | 中国中煤能源集团有限公司 | Decarbonization and desulfurization method for mixed gas containing combustible gas |
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