CN115466609B - Solid slow-release sulfur remover and preparation method thereof - Google Patents
Solid slow-release sulfur remover and preparation method thereof Download PDFInfo
- Publication number
- CN115466609B CN115466609B CN202211113106.3A CN202211113106A CN115466609B CN 115466609 B CN115466609 B CN 115466609B CN 202211113106 A CN202211113106 A CN 202211113106A CN 115466609 B CN115466609 B CN 115466609B
- Authority
- CN
- China
- Prior art keywords
- stirring
- temperature
- heating
- sulfur
- reactor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/54—Compositions for in situ inhibition of corrosion in boreholes or wells
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/52—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
- C09K8/528—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning inorganic depositions, e.g. sulfates or carbonates
- C09K8/532—Sulfur
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/20—Hydrogen sulfide elimination
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Abstract
The invention belongs to the technical field of underground sulfur removal of oil and gas wells, and discloses a solid slow-release sulfur removal agent which comprises the following components in percentage by weight: sulfur removal body: 50-70%; an adhesive: 1-5%; reinforcing agent: 5-10%; the balance of the molding agent; the preparation method of the solid slow-release sulfur remover comprises the following steps: adding the sulfur removal body into a reactor, heating to 80 ℃, stirring the sulfur removal body for 20-30 min, adding the reinforcing agent, stirring for 20-30 min, adding the forming agent, stirring for 10-20 min, and finally adding the adhesive, stirring for 30-40 min; heating the reactor to 100 ℃, when the temperature is raised to 100 ℃, starting vacuumizing, reacting for 30-40 min, stopping heating the reactor, and reducing the temperature to 90-95 ℃ and keeping constant; and conveying the materials in the reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 90-95 ℃, and extruding and granulating by the double-screw extruder to obtain the solid slow-release sulfur remover.
Description
Technical Field
The invention relates to the technical field of underground sulfur removal of oil and gas wells, in particular to a solid slow-release sulfur removal agent and a preparation method thereof.
Background
In the oil gas exploitation process, most oil fields contain hydrogen sulfide to a certain extent, wherein the hydrogen sulfide is colorless and contains extremely toxic strong acid gas, and the hydrogen sulfide is seriously harmful to human bodies through respiratory nervous systems of the human bodies; hydrogen sulfide can cause cracking of metal materials to generate brittle failure through corrosion, and the equipment is endangered; the hydrogen sulfide also can pollute the atmosphere and water and cause harm to water body organisms, animals and plants. Increasingly, different quality oil and gas resources are exploited domestically. In the oil and gas produced, the hydrogen sulfide gas with various concentrations is not contained. The presence of hydrogen sulfide not only seriously threatens the safety of production personnel, but also can cause serious corrosion to production equipment, leading to safety accidents and increased production cost.
The prior sulfur removal process for reducing the hydrogen sulfide applied to the oil gas drilling operation is mainly carried out in the following two modes, namely (1) the liquid discharge operation of the open-flow nozzle and the well control operation, the open fire is ignited at the open-flow nozzle, the hydrogen sulfide gas is combusted, and the timely combustion of the hydrogen sulfide gas in the gas is ensured. (2) In the production process, a sulfur removing device and a sulfur removing agent are arranged, a mixing nipple is arranged on an outlet pipeline of the separator, and the sulfur removing agent is added to remove hydrogen sulfide in the liquid. The main problems are that the open flow and well control operation belongs to a non-production stage, hydrogen sulfide can be combusted, and the hydrogen sulfide cannot be separated and combusted in a normal production period; the liquid sulfur remover has wide application range, but needs injection equipment and places, increases the operation cost, can not be added into stratum, mainly comprises active ferric oxide, zinc oxide and basic carbonate, is mainly used for gas desulfurization in a desulfurizing tower and also used for sulfur removal in drilling fluid, but has no slow release effect, needs continuous addition, is difficult to desulfurize with liquid in process, and therefore, needs to develop an efficient and quick solution for sulfur removal aiming at hydrogen sulfide in the production process of high sulfur-containing oil and gas wells, improves the production efficiency and meets the production requirement of the sulfur-containing oil and gas wells.
Chinese patent No. CN 102698576A, 10/3 in 2012 discloses a sulfur scavenger suitable for use in oil and gas well production, which comprises the following components in mass ratio: 10-25% of hydroxyethyl hexahydro s-triazine, 5-20% of alcohol amine, and 5-20% of small molecular alcohol. The formula is simple, the sulfur removing agent is mutually soluble with water, hydrogen sulfide in crude oil or natural gas can be effectively reduced, the hydrogen sulfide amount in crude oil or weather can be less than 2ppm, and meanwhile, a product formed by the sulfur removing agent and the hydrogen sulfide is dissolved in water, so that a shaft is not blocked, and normal production of an oil-gas well is not influenced; the sulfur scavenger can act within the temperature range of 30-120 ℃ and react with hydrogen sulfide rapidly. Chinese patent No. CN104629700a, 5 months and 20 days 2015 discloses a sulfur removing agent for water producing oil well and water producing gas well, which comprises the following components in percentage by weight: 30-60% of one or more than two of primary amine or secondary amine compounds, alcohol amine compounds and pyridine compounds, and 5-20% of alcohol; finally, the mixture is filled up to 100% by water. The sulfur remover is easy to obtain, nontoxic, reasonable in price, convenient to transport, simple in site construction and free from corroding oil and gas well production pipelines and instruments. And is a liquid adsorption type sulfur removing agent, and reacts with hydrogen sulfide in oil, gas and water in a neutralization chemical way to rapidly remove the hydrogen sulfide in oil gas and sewage in the production process.
The sulfur removing agent represented by the above patent is mainly a liquid sulfur removing agent, mainly alkanolamine and nitrogen-containing sulfur removing agent, and has good application effect, but needs injection equipment and adding operation, increases the running cost, can not be directly added into stratum for slow release, and also has the problems of low absorption capacity and poor high temperature resistance. Aiming at sulfur-containing oil and gas wells, in order to increase the slow release in the stratum to reduce the hydrogen sulfide and improve the long-acting performance of measures, the underground desulfurization of the oil and gas wells in the whole production process is achieved to reduce the consumption of non-production time, and a solid slow release sulfur remover formula is necessary to be developed to meet the long-term sulfur removal requirement of the oil and gas wells.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a solid slow-release sulfur removal agent and a preparation method thereof. The dissolution slow-release time length of the solid desulfurizing agent can reach 200 days when the solid desulfurizing agent is used for desulfurizing under stratum conditions, continuous addition is avoided, and injection equipment is not required to be additionally added, so that the cost is greatly reduced.
The invention aims at realizing the following technical scheme:
the solid slow release sulfur remover comprises the following components in percentage by weight:
sulfur removal body: 50-70%;
an adhesive: 1-5%;
reinforcing agent: 5-10%;
the balance being a forming agent.
Preferably, the sulfur removal body is one or more of hexamethylenetetramine, trioxymethylene and ethylene glycol dimethyl ether.
Preferably, the adhesive is two or three of paraformaldehyde, beta-cyclodextrin and polyethylene glycol.
Preferably, the enhancer is one or more of diglycolamine and 2-methylaminoethanol.
Preferably, the forming agent is one or more of poly (butylene adipate-terephthalate), poly (vinyl alcohol), and poly (p-dioxanone).
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding a sulfur removal body into a reactor, heating to 80 ℃, firstly stirring the sulfur removal body for 20-30 min, then adding an enhancer, stirring for 20-30 min, then adding a forming agent, stirring for 10-20 min, and finally adding an adhesive, stirring for 30-40 min;
step two, heating the reactor to 100 ℃, when the temperature is raised to 100 ℃, starting vacuumizing, reacting for 30-40 min, stopping heating the reactor, and reducing the temperature to 90-95 ℃ and keeping constant;
And thirdly, conveying the materials in the reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 90-95 ℃, and extruding and granulating by the double-screw extruder to obtain the solid slow-release sulfur remover.
Preferably, in the second step, the temperature rising speed is controlled to be 1-2 ℃/min during the temperature rising.
Preferably, in the second step, vacuum is pumped until the pressure is 0.8-0.9 MPa.
Preferably, in the second step, the cooling speed is controlled to be 0.5-1.0 ℃/min during cooling.
Preferably, the solid slow release sulfur removal agent is screened through a screen to control the diameter and length of the material.
Preferably, in the third step, the mixture is sieved with a sieve of 1 to 3. 3 mm.
The beneficial effects of this technical scheme are as follows:
1. the solid slow-release sulfur remover provided by the invention has good slow-release performance. The solid slow-release sulfur removing agent provided by the invention has the advantages that the poly (butylene adipate-terephthalate), the polyvinyl alcohol and the poly (p-dioxanone) are slowly dissolved under the condition of formation water, and the hexamethylene tetramine, the trioxymethylene, the paraformaldehyde and the ethylene glycol dimethyl ether can be slowly released, so that the reactive aldehyde groups are provided, the removal of hydrogen sulfide is realized, the slow release of the solid sulfur removing agent is facilitated, and the effective period is long. The dissolution slow-release time length of the solid desulfurizing agent can reach 200 days when the solid desulfurizing agent is used for desulfurizing under stratum conditions, continuous addition is avoided, and injection equipment is not required to be additionally added, so that the cost is greatly reduced.
2. The solid slow-release sulfur remover provided by the invention has the advantages of controllable particle size and convenience in transportation. The solid slow-release sulfur remover can be processed into solid particles with different particle sizes according to the process requirements, and compared with liquid, the solid slow-release sulfur remover is convenient to transport.
3. The solid slow-release sulfur remover provided by the invention has high compressive strength and is added in a compound way. The solid slow-release sulfur remover has higher compressive strength, can be carried into a stratum in the fracturing and acidizing processes, can be used as a diversion agent in the process, improves the measure effect, and can also be used as a conventional solid sulfur remover.
4. The solid slow-release sulfur remover provided by the invention is suitable for removing hydrogen sulfide from gas or liquid. The solid slow release sulfur remover can be used for gas desulfurization and liquid desulfurization.
5. The solid slow-release sulfur remover provided by the invention does not contain metal ions. The solid slow release sulfur removing agent does not contain any metal ions such as calcium, magnesium, iron and the like, and forms metal ion sediment under the condition of no stratum to pollute the stratum.
6. The invention provides a solid slow-release sulfur remover, which is used for underground desulfurization. The solid slow-release sulfur remover provided by the invention has the characteristics of high efficiency, long time and the like when being used for desulfurizing under stratum conditions.
7. According to the preparation method of the solid slow-release sulfur remover, provided by the invention, the liquid and the solid in the formula are fully mixed, so that conditions are created for subsequent granulation; vacuumizing to prevent bubbles from being mixed in particles, so that the compression resistance and other performances of the product are affected; the double-screw extruder can be used for manufacturing the product into granular solid, so that the particle size and compression resistance requirements of the product are met.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto.
It is noted that when an element is referred to as being "mounted," "secured," or "disposed" on another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or intervening elements may also be present.
It should be noted that, in the embodiments of the present invention, terms such as left, right, up, and down are merely relative concepts or references to normal use states of the product, and should not be construed as limiting.
Example 1
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 70% of a sulfur removal body; 5% of an adhesive; 8% of reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal body consists of 50 weight percent of hexamethylenetetramine, 25 weight percent of trioxymethylene and 25 weight percent of ethylene glycol dimethyl ether; the adhesive consists of 20 weight percent of paraformaldehyde, 70 weight percent of beta-cyclodextrin and 10 weight percent of polyethylene glycol; the reinforcing agent consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylaminoethanol; the molding agent consists of 70% by weight of poly (butylene adipate-terephthalate), 15% of polyvinyl alcohol and 15% of poly (p-dioxanone).
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding a formula amount of sulfur removal body into an intermittent stirring reactor, heating to 80 ℃, firstly adding the formula amount of sulfur removal body, stirring for 20 min, then adding the formula amount of reinforcing agent, stirring for 20 min, then adding the formula amount of forming agent, stirring for 10 min, and finally adding the formula amount of adhesive, stirring for 30 min;
step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 1 ℃/min, starting vacuumizing (vacuumizing to 0.8 MPa) when the temperature is increased to 100 ℃, reacting for 30 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 0.5 ℃/min, and reducing the temperature to 90 ℃ and keeping constant;
And thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 90 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 1-1.8 mm to control the diameter and length of the materials, thereby obtaining the solid slow-release sulfur remover.
Example 2
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 50% of a sulfur removal body; 5% of an adhesive; 10% of reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal body consists of 50 weight percent of hexamethylenetetramine and 50 weight percent of trioxymethylene; the adhesive consists of 70% by weight of paraformaldehyde and 30% by weight of beta-cyclodextrin; the reinforcing agent consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylaminoethanol; the molding agent consists of 70% by weight of poly (butylene adipate-terephthalate), 15% of polyvinyl alcohol and 15% of poly (p-dioxanone).
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding the bulk of the formula amount into an intermittent stirring reactor, heating to 80 ℃, adding the bulk of the formula amount, stirring for 25 min, adding the reinforcing agent of the formula amount, stirring for 25 min, adding the forming agent of the formula amount, stirring for 15 min, and finally adding the adhesive of the formula amount, stirring for 35 min;
Step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 1.5 ℃/min, starting vacuumizing (vacuumizing to 0.85 MPa) when the temperature is increased to 100 ℃, reacting for 35 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 0.75 ℃/min, and reducing the temperature to 92.5 ℃ and keeping constant;
and thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 92.5 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen with the diameter and the length of 1.8-2.4mm to obtain the solid slow-release sulfur remover.
Example 3
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 60% of a sulfur removal body; 3% of an adhesive; 5% of a reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal body consists of 30 weight percent of hexamethylenetetramine, 57 weight percent of trioxymethylene and 13 weight percent of ethylene glycol dimethyl ether; the adhesive consists of 65 weight percent of paraformaldehyde and 35 weight percent of beta-cyclodextrin; the reinforcing agent consists of diglycolamine; the molding agent consists of 70% by weight of poly (butylene adipate-terephthalate) and 30% by weight of polyvinyl alcohol.
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding the bulk of the formula amount into an intermittent stirring reactor, heating to 80 ℃, adding the bulk of the formula amount, stirring for 30 min, adding the reinforcing agent of the formula amount, stirring for 30 min, adding the forming agent of the formula amount, stirring for 20 min, and finally adding the adhesive of the formula amount, stirring for 40 min;
step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 2 ℃/min, starting vacuumizing (vacuumizing to 0.9 MPa) when the temperature is increased to 100 ℃, reacting for 40 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 1 ℃/min, and reducing the temperature to 95 ℃ and keeping constant;
and thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 95 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 2.4-3 mm to control the diameter and length of the materials, thereby obtaining the solid slow-release sulfur remover.
Example 4
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 55% of a sulfur removal body; 3% of an adhesive; 5% of a reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal body consists of 80 weight percent of trioxymethylene and 20 weight percent of ethylene glycol dimethyl ether; the adhesive consists of 70 weight percent of paraformaldehyde and 30 weight percent of polyethylene glycol; the reinforcing agent consists of 2-methylaminoethanol; the molding agent consists of 70% by weight of polybutylene adipate-terephthalate, 10% of polyvinyl alcohol and 20% of polydioxanone.
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding the bulk of the formula amount into an intermittent stirring reactor, heating to 80 ℃, adding the bulk of the formula amount, stirring for 30 min, adding the reinforcing agent of the formula amount, stirring for 30 min, adding the forming agent of the formula amount, stirring for 20 min, and finally adding the adhesive of the formula amount, stirring for 40 min;
step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 2 ℃/min, starting vacuumizing (vacuumizing to 0.8 MPa) when the temperature is increased to 100 ℃, reacting for 40 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 1 ℃/min, and reducing the temperature to 95 ℃ and keeping constant;
and thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 95 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 2.4-3 mm to control the diameter and length of the materials, thereby obtaining the solid slow-release sulfur remover.
Example 5
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 60% of a sulfur removal body; 1% of an adhesive; 8% of reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal bulk consists of 100 percent by weight of hexamethylenetetramine; the adhesive consists of 70 weight percent of paraformaldehyde and 30 weight percent of polyethylene glycol; the reinforcing agent consists of 2-methylaminoethanol; the molding agent consists of 70% by weight of polybutylene adipate-terephthalate, 10% of polyvinyl alcohol and 20% of polydioxanone.
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding the bulk of the formula amount into an intermittent stirring reactor, heating to 80 ℃, adding the bulk of the formula amount, stirring for 30 min, adding the reinforcing agent of the formula amount, stirring for 30 min, adding the forming agent of the formula amount, stirring for 20 min, and finally adding the adhesive of the formula amount, stirring for 40 min;
step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 2 ℃/min, starting vacuumizing (vacuumizing to 0.9 MPa) when the temperature is increased to 100 ℃, reacting for 40 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 1 ℃/min, and reducing the temperature to 95 ℃ and keeping constant;
And thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 95 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 2.4-3 mm to control the diameter and length of the materials, thereby obtaining the solid slow-release sulfur remover.
Comparative example 1
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 75% of a sulfur removal body; 5% of an adhesive; 8% of reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal body consists of 50 weight percent of hexamethylenetetramine, 25 weight percent of trioxymethylene and 25 weight percent of ethylene glycol dimethyl ether; the adhesive consists of 20 weight percent of paraformaldehyde, 70 weight percent of beta-cyclodextrin and 10 weight percent of polyethylene glycol; the reinforcing agent consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylaminoethanol; the molding agent consists of 70% by weight of poly (butylene adipate-terephthalate), 15% of polyvinyl alcohol and 15% of poly (p-dioxanone).
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding a formula amount of sulfur removal body into an intermittent stirring reactor, heating to 80 ℃, firstly adding the formula amount of sulfur removal body, stirring for 20 min, then adding the formula amount of reinforcing agent, stirring for 20 min, then adding the formula amount of forming agent, stirring for 10 min, and finally adding the formula amount of adhesive, stirring for 30 min;
Step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 1 ℃/min, starting vacuumizing (vacuumizing to 0.8 MPa) when the temperature is increased to 100 ℃, reacting for 30 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 0.5 ℃/min, and reducing the temperature to 90 ℃ and keeping constant;
and thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 90 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 1-1.8 mm to control the diameter and length of the materials, thereby obtaining the solid slow-release sulfur remover.
Comparative example 2
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 70% of a sulfur removal body; 6% of an adhesive; 8% of reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal body consists of 50 weight percent of hexamethylenetetramine, 25 weight percent of trioxymethylene and 25 weight percent of ethylene glycol dimethyl ether; the adhesive consists of 20 weight percent of paraformaldehyde, 70 weight percent of beta-cyclodextrin and 10 weight percent of polyethylene glycol; the reinforcing agent consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylaminoethanol; the molding agent consists of 70% by weight of poly (butylene adipate-terephthalate), 15% of polyvinyl alcohol and 15% of poly (p-dioxanone).
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding a formula amount of sulfur removal body into an intermittent stirring reactor, heating to 80 ℃, firstly adding the formula amount of sulfur removal body, stirring for 20 min, then adding the formula amount of reinforcing agent, stirring for 20 min, then adding the formula amount of forming agent, stirring for 10 min, and finally adding the formula amount of adhesive, stirring for 30 min;
step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 1 ℃/min, starting vacuumizing (vacuumizing to 0.8 MPa) when the temperature is increased to 100 ℃, reacting for 30 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 0.5 ℃/min, and reducing the temperature to 90 ℃ and keeping constant;
and thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 90 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 1-1.8 mm to control the diameter and length of the materials, thereby obtaining the solid slow-release sulfur remover.
Comparative example 3
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 70% of a sulfur removal body; 5% of an adhesive; 12% of reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal body consists of 50 weight percent of hexamethylenetetramine, 25 weight percent of trioxymethylene and 25 weight percent of ethylene glycol dimethyl ether; the adhesive consists of 20 weight percent of paraformaldehyde, 70 weight percent of beta-cyclodextrin and 10 weight percent of polyethylene glycol; the reinforcing agent consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylaminoethanol; the molding agent consists of 70% by weight of poly (butylene adipate-terephthalate), 15% of polyvinyl alcohol and 15% of poly (p-dioxanone).
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding a formula amount of sulfur removal body into an intermittent stirring reactor, heating to 80 ℃, firstly adding the formula amount of sulfur removal body, stirring for 20 min, then adding the formula amount of reinforcing agent, stirring for 20 min, then adding the formula amount of forming agent, stirring for 10 min, and finally adding the formula amount of adhesive, stirring for 30 min;
step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 1 ℃/min, starting vacuumizing (vacuumizing to 0.8 MPa) when the temperature is increased to 100 ℃, reacting for 30 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 0.5 ℃/min, and reducing the temperature to 90 ℃ and keeping constant;
And thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 90 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 1-1.8 mm to control the diameter and length of the materials, thereby obtaining the solid slow-release sulfur remover.
Comparative example 4
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 45% of a sulfur removal body; 5% of an adhesive; 10% of reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal body consists of 50 weight percent of hexamethylenetetramine and 50 weight percent of trioxymethylene; the adhesive consists of 70% by weight of paraformaldehyde and 30% by weight of beta-cyclodextrin; the reinforcing agent consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylaminoethanol; the molding agent consists of 70% by weight of poly (butylene adipate-terephthalate), 15% of polyvinyl alcohol and 15% of poly (p-dioxanone).
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding the bulk of the formula amount into an intermittent stirring reactor, heating to 80 ℃, adding the bulk of the formula amount, stirring for 25 min, adding the reinforcing agent of the formula amount, stirring for 25 min, adding the forming agent of the formula amount, stirring for 15 min, and finally adding the adhesive of the formula amount, stirring for 35 min;
Step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 1.5 ℃/min, starting vacuumizing (vacuumizing to 0.85 MPa) when the temperature is increased to 100 ℃, reacting for 35 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 0.75 ℃/min, and reducing the temperature to 92.5 ℃ and keeping constant;
and thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 92.5 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen with the diameter and the length of 1.8-2.4mm to obtain the solid slow-release sulfur remover.
Comparative example 5
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 50% of a sulfur removal body; 0.5% of adhesive; 10% of reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal body consists of 50 weight percent of hexamethylenetetramine and 50 weight percent of trioxymethylene; the adhesive consists of 70% by weight of paraformaldehyde and 30% by weight of beta-cyclodextrin; the reinforcing agent consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylaminoethanol; the molding agent consists of 70% by weight of poly (butylene adipate-terephthalate), 15% of polyvinyl alcohol and 15% of poly (p-dioxanone).
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding the bulk of the formula amount into an intermittent stirring reactor, heating to 80 ℃, adding the bulk of the formula amount, stirring for 25 min, adding the reinforcing agent of the formula amount, stirring for 25 min, adding the forming agent of the formula amount, stirring for 15 min, and finally adding the adhesive of the formula amount, stirring for 35 min;
step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 1.5 ℃/min, starting vacuumizing (vacuumizing to 0.85 MPa) when the temperature is increased to 100 ℃, reacting for 35 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 0.75 ℃/min, and reducing the temperature to 92.5 ℃ and keeping constant;
and thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 92.5 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen with the diameter and the length of 1.8-2.4mm to obtain the solid slow-release sulfur remover.
Comparative example 6
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 50% of a sulfur removal body; 5% of an adhesive; 4% of reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal body consists of 50 weight percent of hexamethylenetetramine and 50 weight percent of trioxymethylene; the adhesive consists of 70% by weight of paraformaldehyde and 30% by weight of beta-cyclodextrin; the reinforcing agent consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylaminoethanol; the molding agent consists of 70% by weight of poly (butylene adipate-terephthalate), 15% of polyvinyl alcohol and 15% of poly (p-dioxanone).
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding the bulk of the formula amount into an intermittent stirring reactor, heating to 80 ℃, adding the bulk of the formula amount, stirring for 25 min, adding the reinforcing agent of the formula amount, stirring for 25 min, adding the forming agent of the formula amount, stirring for 15 min, and finally adding the adhesive of the formula amount, stirring for 35 min;
step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 1.5 ℃/min, starting vacuumizing (vacuumizing to 0.85 MPa) when the temperature is increased to 100 ℃, reacting for 35 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 0.75 ℃/min, and reducing the temperature to 92.5 ℃ and keeping constant;
and thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 92.5 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen with the diameter and the length of 1.8-2.4mm to obtain the solid slow-release sulfur remover.
Comparative example 7
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 60% of a sulfur removal body; 3% of an adhesive; 5% of a reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal body consists of 30 weight percent of hexamethylenetetramine, 57 weight percent of trioxymethylene and 13 weight percent of ethylene glycol dimethyl ether; the adhesive consists of 65 weight percent of paraformaldehyde and 35 weight percent of beta-cyclodextrin; the reinforcing agent consists of diglycolamine; the molding agent consists of 70% by weight of poly (butylene adipate-terephthalate) and 30% by weight of polyvinyl alcohol.
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding the bulk of the formula amount into an intermittent stirring reactor, heating to 75 ℃, adding the bulk of the formula amount, stirring for 30 min, adding the reinforcing agent of the formula amount, stirring for 30 min, adding the forming agent of the formula amount, stirring for 20 min, and finally adding the adhesive of the formula amount, stirring for 40 min;
step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 2 ℃/min, starting vacuumizing (vacuumizing to 0.9 MPa) when the temperature is increased to 100 ℃, reacting for 40 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 1 ℃/min, and reducing the temperature to 95 ℃ and keeping constant;
And thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 95 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 2.4-3 mm to control the diameter and length of the materials, thereby obtaining the solid slow-release sulfur remover.
Comparative example 8
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 60% of a sulfur removal body; 3% of an adhesive; 5% of a reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal body consists of 30 weight percent of hexamethylenetetramine, 57 weight percent of trioxymethylene and 13 weight percent of ethylene glycol dimethyl ether; the adhesive consists of 65 weight percent of paraformaldehyde and 35 weight percent of beta-cyclodextrin; the reinforcing agent consists of diglycolamine; the molding agent consists of 70% by weight of poly (butylene adipate-terephthalate) and 30% by weight of polyvinyl alcohol.
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding the bulk of the formula amount into an intermittent stirring reactor, heating to 85 ℃, adding the bulk of the formula amount, stirring for 30 min, adding the reinforcing agent of the formula amount, stirring for 30 min, adding the forming agent of the formula amount, stirring for 20 min, and finally adding the adhesive of the formula amount, stirring for 40 min;
Step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 2 ℃/min, starting vacuumizing (vacuumizing to 0.9 MPa) when the temperature is increased to 100 ℃, reacting for 40 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 1 ℃/min, and reducing the temperature to 95 ℃ and keeping constant;
and thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 95 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 2.4-3 mm to control the diameter and length of the materials, thereby obtaining the solid slow-release sulfur remover.
Comparative example 9
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 55% of a sulfur removal body; 3% of an adhesive; 5% of a reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal body consists of 80 weight percent of trioxymethylene and 20 weight percent of ethylene glycol dimethyl ether; the adhesive consists of 70 weight percent of paraformaldehyde and 30 weight percent of polyethylene glycol; the reinforcing agent consists of 2-methylaminoethanol; the molding agent consists of 70% by weight of polybutylene adipate-terephthalate, 10% of polyvinyl alcohol and 20% of polydioxanone.
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding the bulk of the formula amount into an intermittent stirring reactor, heating to 80 ℃, adding the bulk of the formula amount, stirring for 30 min, adding the reinforcing agent of the formula amount, stirring for 30 min, adding the forming agent of the formula amount, stirring for 20 min, and finally adding the adhesive of the formula amount, stirring for 40 min;
step two, heating the intermittent stirring reactor to 95 ℃, controlling the heating speed to be 2 ℃/min, starting vacuumizing (vacuumizing to 0.8 MPa) when the temperature is increased to 95 ℃, reacting for 40 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 1 ℃/min, and reducing the temperature to be 85 ℃ and keeping constant;
and thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 85 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 2.4-3 mm to control the diameter and length of the materials, thereby obtaining the solid slow-release sulfur remover.
Comparative example 10
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 55% of a sulfur removal body; 3% of an adhesive; 5% of a reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal body consists of 80 weight percent of trioxymethylene and 20 weight percent of ethylene glycol dimethyl ether; the adhesive consists of 70 weight percent of paraformaldehyde and 30 weight percent of polyethylene glycol; the reinforcing agent consists of 2-methylaminoethanol; the molding agent consists of 70% by weight of polybutylene adipate-terephthalate, 10% of polyvinyl alcohol and 20% of polydioxanone.
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding the bulk of the formula amount into an intermittent stirring reactor, heating to 110 ℃, adding the bulk of the formula amount, stirring for 30 min, adding the reinforcing agent of the formula amount, stirring for 30 min, adding the forming agent of the formula amount, stirring for 20 min, and finally adding the adhesive of the formula amount, stirring for 40 min;
step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 2 ℃/min, starting vacuumizing (vacuumizing to 0.8 MPa) when the temperature is increased to 100 ℃, reacting for 40 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 1 ℃/min, and reducing the temperature to 85 ℃ and keeping constant;
and thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 100 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 2.4-3 mm to control the diameter and length of the materials, thereby obtaining the solid slow-release sulfur remover.
Comparative example 11
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 60% of a sulfur removal body; 1% of an adhesive; 8% of reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal bulk consists of 100 percent by weight of hexamethylenetetramine; the adhesive consists of 70 weight percent of paraformaldehyde and 30 weight percent of polyethylene glycol; the reinforcing agent consists of 2-methylaminoethanol; the molding agent consists of 70% by weight of polybutylene adipate-terephthalate, 10% of polyvinyl alcohol and 20% of polydioxanone.
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding the bulk of the formula amount into an intermittent stirring reactor, heating to 80 ℃, adding the bulk of the formula amount, stirring for 30 min, adding the reinforcing agent of the formula amount, stirring for 30 min, adding the forming agent of the formula amount, stirring for 20 min, and finally adding the adhesive of the formula amount, stirring for 40 min;
step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 2.5 ℃/min, starting vacuumizing (vacuumizing to 0.9 MPa) when the temperature is increased to 100 ℃, reacting for 40 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 1.5 ℃/min, and reducing the temperature to 95 ℃ and keeping constant;
And thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 95 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 2.4-3 mm to control the diameter and length of the materials, thereby obtaining the solid slow-release sulfur remover.
Comparative example 12
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 60% of a sulfur removal body; 1% of an adhesive; 8% of reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal bulk consists of 100 percent by weight of hexamethylenetetramine; the adhesive consists of 70 weight percent of paraformaldehyde and 30 weight percent of polyethylene glycol; the reinforcing agent consists of 2-methylaminoethanol; the molding agent consists of 70% by weight of polybutylene adipate-terephthalate, 10% of polyvinyl alcohol and 20% of polydioxanone.
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding the bulk of the formula amount into an intermittent stirring reactor, heating to 80 ℃, adding the bulk of the formula amount, stirring for 30 min, adding the reinforcing agent of the formula amount, stirring for 30 min, adding the forming agent of the formula amount, stirring for 20 min, and finally adding the adhesive of the formula amount, stirring for 40 min;
Step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 0.5 ℃/min, starting vacuumizing (vacuumizing to 0.9 MPa) when the temperature is increased to 100 ℃, reacting for 40 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 0.25 ℃/min, and reducing the temperature to 95 ℃ and keeping constant;
and thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 95 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 2.4-3 mm to control the diameter and length of the materials, thereby obtaining the solid slow-release sulfur remover.
Comparative example 13
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 70% of a sulfur removal body; 5% of an adhesive; 8% of reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal body consists of 50 weight percent of hexamethylenetetramine, 25 weight percent of trioxymethylene and 25 weight percent of ethylene glycol dimethyl ether; the adhesive consists of 20 weight percent of paraformaldehyde, 70 weight percent of beta-cyclodextrin and 10 weight percent of polyethylene glycol; the reinforcing agent consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylaminoethanol; the molding agent consists of 70% by weight of poly (butylene adipate-terephthalate), 15% of polyvinyl alcohol and 15% of poly (p-dioxanone).
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding a formula amount of sulfur removal body into an intermittent stirring reactor, heating to 80 ℃, firstly adding the formula amount of sulfur removal body, stirring for 20 min, then adding the formula amount of reinforcing agent, stirring for 20 min, then adding the formula amount of forming agent, stirring for 10 min, and finally adding the formula amount of adhesive, stirring for 30 min;
step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 1 ℃/min, starting vacuumizing (vacuumizing to 0.75 MPa) when the temperature is increased to 100 ℃, reacting for 30 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 0.5 ℃/min, and reducing the temperature to 90 ℃ and keeping constant;
and thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 90 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 1-1.8 mm to control the diameter and length of the materials, thereby obtaining the solid slow-release sulfur remover.
Comparative example 14
The invention discloses a solid slow-release sulfur remover, which comprises the following components in percentage by weight: 70% of a sulfur removal body; 5% of an adhesive; 8% of reinforcing agent; the balance being a forming agent.
Wherein: the sulfur removal body consists of 50 weight percent of hexamethylenetetramine, 25 weight percent of trioxymethylene and 25 weight percent of ethylene glycol dimethyl ether; the adhesive consists of 20 weight percent of paraformaldehyde, 70 weight percent of beta-cyclodextrin and 10 weight percent of polyethylene glycol; the reinforcing agent consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylaminoethanol; the molding agent consists of 70% by weight of poly (butylene adipate-terephthalate), 15% of polyvinyl alcohol and 15% of poly (p-dioxanone).
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding a formula amount of sulfur removal body into an intermittent stirring reactor, heating to 80 ℃, firstly adding the formula amount of sulfur removal body, stirring for 20 min, then adding the formula amount of reinforcing agent, stirring for 20 min, then adding the formula amount of forming agent, stirring for 10 min, and finally adding the formula amount of adhesive, stirring for 30 min;
step two, heating the intermittent stirring reactor to 100 ℃, controlling the heating speed to be 1 ℃/min, starting vacuumizing (vacuumizing to 0.95 MPa) when the temperature is increased to 100 ℃, reacting for 30 min, stopping heating the intermittent stirring reactor, controlling the cooling speed to be 0.5 ℃/min, and reducing the temperature to 90 ℃ and keeping constant;
And thirdly, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 90 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 1-1.8 mm to control the diameter and length of the materials, thereby obtaining the solid slow-release sulfur remover.
The solid slow release sulfur scavengers obtained in examples 1 to 5 and comparative examples 1 to 14 were subjected to water dissolution test, hydrogen sulfide absorption performance test and pressure test at different temperatures.
1. And (5) dissolution testing.
Taking 1 g solid slow-release sulfur removing agent (particle size range of 1-3 mm), placing in a test tube with a plug, pouring 100 mL distilled water, placing in a 65 ℃ water bath kettle, filtering after 24 hours, adding 100 ml distilled water again into the solid on the filter paper, continuously measuring the dissolution amount in different time periods, repeating the steps, and calculating the dissolution rate.
2. Hydrogen sulfide absorption performance test
1.0 mL hydrochloric acid solution was removed, placed in a 15 mL plastic test tube, and transferred to a 500 mL anaerobic jar. Adding 0.5 mL sodium sulfide solution into the plastic test tube, rapidly covering the anaerobic bottle plug, shaking the bottle body for 10 weeks, placing in a 60 ℃ oven, and shaking the bottle body for 10 weeks every 5 min. 20 After min, the filtrate in different time periods in the dissolution test is injected into the bottom of the anaerobic bottle and is shaken The body was moved for 10 weeks and placed in an oven at 60 ℃.30 After min, H in the bottle is detected by a gas detection hand pump and a hydrogen sulfide detection tube 2 S gas content and reading, and simultaneously performing a blank experiment, wherein H in the bottle is detected by using a gas detection hand pump and a hydrogen sulfide detection tube for the blank experiment 2 S gas content and reading. After the experiment was completed, the anaerobic jar was placed in a fume hood and residual hydrogen sulfide gas was absorbed with excess sodium hydroxide solution. And calculating the sulfur removal rate according to the content change of the hydrogen sulfide gas passing through the inlet and the outlet of the absorption bottle.
X=(C1-C2) *100/C1
Wherein: x-desulfurization percentage,% (sulfur removal time: 5 min)
Hydrogen sulfide content in C1-blank experiments, ppm
C2 Determination of the Hydrogen sulfide content in the experiments, ppm
3. And (5) bearing test.
Taking a solid slow-release sulfur removing agent (the grain size range is 1-3 mm), testing the crushing rate in a press, wherein the crushing rate is extremely low when the pressure is within 10 MPa, the average crushing rate is about 3%, and the pressure resistance is measured under the condition of 10% of the crushing rate.
The percent of dissolution (%) of the qualified product is 10 d: 0.05-0.15, 100d dissolution rate (%): 45-50, 200d dissolution rate (%) 96-100, 10d sulfur removal rate (%) is more than or equal to 98; the sulfur removal rate (%) is more than or equal to 99 after 100 d; 200d sulfur removal rate (%) =100; the pressure bearing (MPa) is more than or equal to 15.
The cleanup additives of examples 1-5 and comparative examples 1-14 were tested for corrosion inhibition, liquid carrying capacity, and scale inhibition, and the data are shown in the following table:
From the examination of examples 1-5 and comparative examples 1-14, it was found that specific sulfur removal bulk, binder, enhancer and molding agent compositions and ratios were required, and specific preparation steps and process parameters were required to obtain acceptable solid slow release sulfur scavengers.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent variation, etc. of the above embodiment according to the technical matter of the present invention fall within the scope of the present invention.
Claims (3)
1. The solid slow release sulfur remover is characterized by comprising the following components in percentage by weight:
sulfur removal body: 50-70%;
an adhesive: 1-5%;
reinforcing agent: 5-10%;
the balance of the molding agent;
the sulfur removal body is one or more of hexamethylenetetramine, trioxymethylene and ethylene glycol dimethyl ether;
the adhesive is two or three of paraformaldehyde, beta-cyclodextrin and polyethylene glycol;
the reinforcing agent is one or more of diglycolamine and 2-methylaminoethanol;
the forming agent is one or more of poly (butylene adipate-terephthalate), polyvinyl alcohol and poly (p-dioxanone);
The preparation method of the solid slow-release sulfur remover comprises the following steps:
step one, adding a sulfur removal body into a reactor, heating to 80 ℃, firstly stirring the sulfur removal body for 20-30 min, then adding an enhancer, stirring for 20-30 min, then adding a forming agent, stirring for 10-20 min, and finally adding an adhesive, stirring for 30-40 min;
step two, heating the temperature of the reactor to 100 ℃, and controlling the heating speed to be 1-2 ℃/min when the temperature is raised; when the temperature is raised to 100 ℃, starting to vacuumize until the pressure is 0.8-0.9 MPa; after reacting for 30-40 min, stopping heating the reactor, reducing the temperature to 90-95 ℃ and keeping constant, and controlling the cooling speed to be 0.5-1.0 ℃/min during the cooling;
and thirdly, conveying the materials in the reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 90-95 ℃, and extruding and granulating by the double-screw extruder to obtain the solid slow-release sulfur remover.
2. The method for preparing a solid sustained-release sulfur remover according to claim 1, comprising the following steps:
step one, adding a sulfur removal body into a reactor, heating to 80 ℃, firstly stirring the sulfur removal body for 20-30 min, then adding an enhancer, stirring for 20-30 min, then adding a forming agent, stirring for 10-20 min, and finally adding an adhesive, stirring for 30-40 min;
Step two, heating the temperature of the reactor to 100 ℃, and controlling the heating speed to be 1-2 ℃/min when the temperature is raised; when the temperature is raised to 100 ℃, starting to vacuumize until the pressure is 0.8-0.9 MPa; after reacting for 30-40 min, stopping heating the reactor, reducing the temperature to 90-95 ℃ and keeping constant, and controlling the cooling speed to be 0.5-1.0 ℃/min during the cooling;
and thirdly, conveying the materials in the reactor to a double-screw extruder, controlling the temperature of the double-screw extruder to be 90-95 ℃, and extruding and granulating by the double-screw extruder to obtain the solid slow-release sulfur remover.
3. The method for preparing the solid sustained-release sulfur remover according to claim 2, wherein the method comprises the following steps: in the third step, the solid slow release sulfur remover is screened by a screen mesh of 1-3 mm to control the diameter and the length of the material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211113106.3A CN115466609B (en) | 2022-09-14 | 2022-09-14 | Solid slow-release sulfur remover and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211113106.3A CN115466609B (en) | 2022-09-14 | 2022-09-14 | Solid slow-release sulfur remover and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115466609A CN115466609A (en) | 2022-12-13 |
| CN115466609B true CN115466609B (en) | 2023-06-30 |
Family
ID=84371238
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211113106.3A Active CN115466609B (en) | 2022-09-14 | 2022-09-14 | Solid slow-release sulfur remover and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115466609B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5688478A (en) * | 1994-08-24 | 1997-11-18 | Crescent Holdings Limited | Method for scavenging sulfides |
| AU1530001A (en) * | 1999-11-18 | 2001-05-30 | Champion Technologies, Inc. | Inhibitor compositions |
| CN104629700A (en) * | 2015-02-03 | 2015-05-20 | 成都理工大学 | Sulfur removal agent for water production oil well and water production gas well |
| CN104941440A (en) * | 2015-06-26 | 2015-09-30 | 新疆新辰鼎盛石油工程有限公司 | Solid sulfur removal agent and preparation method thereof |
| EP3505591A1 (en) * | 2018-01-02 | 2019-07-03 | Clariant International Ltd | Synergized acetals composition and method for scavenging sulfides and mercaptans |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019028400A1 (en) * | 2017-08-03 | 2019-02-07 | Ecolab Usa Inc. | Thiol adducts for corrosion inhibition |
-
2022
- 2022-09-14 CN CN202211113106.3A patent/CN115466609B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5688478A (en) * | 1994-08-24 | 1997-11-18 | Crescent Holdings Limited | Method for scavenging sulfides |
| AU1530001A (en) * | 1999-11-18 | 2001-05-30 | Champion Technologies, Inc. | Inhibitor compositions |
| CN104629700A (en) * | 2015-02-03 | 2015-05-20 | 成都理工大学 | Sulfur removal agent for water production oil well and water production gas well |
| CN104941440A (en) * | 2015-06-26 | 2015-09-30 | 新疆新辰鼎盛石油工程有限公司 | Solid sulfur removal agent and preparation method thereof |
| EP3505591A1 (en) * | 2018-01-02 | 2019-07-03 | Clariant International Ltd | Synergized acetals composition and method for scavenging sulfides and mercaptans |
Non-Patent Citations (2)
| Title |
|---|
| Sorbents for hydrogen sulfide capture from biogas at low temperature: a review;Dongjing Liu等;《Environmental Chemistry Letters》(第第18期期);第113-128页 * |
| 海上油田"键桥"型防沉淀液体除硫剂的研究与应用;常振等;《精细石油化工》;第39卷(第2期);第37-41页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115466609A (en) | 2022-12-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US10543448B2 (en) | Agglomeration-resistant desulfurizing product | |
| CN111265993B (en) | Complex iron desulfurizer | |
| KR101333141B1 (en) | Functional fluid and a process for the preparation of the functional fluid | |
| CN111057060B (en) | Synthesis process of composite piperazine heavy metal chelating agent TDDP | |
| CN107857674B (en) | Oyster shell soil repairing agent and preparation method thereof | |
| CN107200385A (en) | A kind of method that iron carbon or Fenton sludge prepare porous light electrolysis particle in utilization waste water treatment process | |
| CN107353929A (en) | A kind of desulfurizing agent and its application | |
| RU2446880C2 (en) | Method and reagent for removing oxygen from hydrocarbon streams | |
| CN115466609B (en) | Solid slow-release sulfur remover and preparation method thereof | |
| CN106381182B (en) | A kind of liquid-absorbant and its application for removing hydrogen sulfide | |
| CN113234473A (en) | Liquid desulfurizing agent for oil field and preparation and application method thereof | |
| KR101774443B1 (en) | Liquid-form catalyst compositions for the removal of hydrogen sulfide from biogas | |
| CN115637168A (en) | High-efficiency composite desulfurizer for oil extraction in oil and gas field | |
| EP3728114B1 (en) | Process for the removal of heavy metals from liquids | |
| CN114395386A (en) | Solid foam water discharging agent with hydrogen sulfide removing function for gas well and preparation method thereof | |
| CN112156610A (en) | Method for effectively removing harmful substances in organic waste liquid combustion flue gas | |
| CN110090850A (en) | It is a kind of using humic acid as the cement solidification arsenic scum method of additive | |
| CN115318098B (en) | Temperature-resistant complex iron desulfurizing agent | |
| CN114425302B (en) | High specific surface area activated carbon gel particles and spray preparation method, application and preparation device thereof | |
| AU2019298824A1 (en) | Creation of an iron product for wastewater treatment | |
| CN114854427B (en) | Attapulgite-based heavy metal ion passivator, preparation method thereof and application thereof in soil remediation | |
| KR101597204B1 (en) | Aqueous desurfurization compositions for the removal of hydrogen sulfide from gaseous streams | |
| CN105536499B (en) | A kind of mercury removal agent and its preparation method and application | |
| CN106635207A (en) | Semi-coke liquor and production process thereof | |
| CN115155513B (en) | Preparation method and application of modified volcanic ash |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |