CN115466609A - Solid slow-release sulfur removal agent and preparation method thereof - Google Patents
Solid slow-release sulfur removal agent and preparation method thereof Download PDFInfo
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- 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
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- 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
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- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
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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: a sulfur removal body: 50-70%; adhesive agent: 1 to 5 percent; reinforcing agent: 5 to 10 percent; the rest is forming agent; a preparation method of a solid slow-release sulfur removal agent 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, and stirring for 30-40 min; heating the reactor to 100 ℃, starting vacuumizing when the temperature is raised to 100 ℃, reacting for 30-40 min, then stopping heating the reactor, and reducing the temperature to 90-95 ℃ and keeping the temperature constant; and (3) conveying the materials in the reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 90-95 ℃, and extruding and granulating by the double-screw extruder to obtain the solid slow-release desulfurizing agent.
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 and gas exploitation process, most oil fields contain hydrogen sulfide to a certain extent, the hydrogen sulfide is colorless and highly toxic strong acid gas, and the hydrogen sulfide can cause serious harm to human bodies through respiratory nervous systems of the human bodies; the hydrogen sulfide can cause the cracking of the metal material to generate brittle failure through corrosion, thereby causing damage to equipment; the hydrogen sulfide can also pollute the atmosphere and water, and cause harm to aquatic organisms and animals and plants. Increasingly, oil and gas resources of different qualities are exploited domestically. The produced oil gas contains no hydrogen sulfide gas with various concentrations. The presence of hydrogen sulfide not only seriously threatens the safety of production personnel, but also seriously corrodes production equipment, resulting in safety accidents and increased production cost.
The existing sulfur removal process for reducing hydrogen sulfide applied to oil and gas drilling operation mainly comprises (1) open-flow liquid drainage operation and well killing operation in the following two modes, wherein open fire is ignited at an open-flow port to burn hydrogen sulfide gas, so that the hydrogen sulfide gas in the gas is ensured to be burned in time. (2) In the production process, a sulfur removal device and a sulfur removal agent are prepared, a mixed short joint is installed on an outlet pipeline of the separator, the sulfur removal agent is added, and hydrogen sulfide in liquid is removed. The main problems existing in the above are that the open flow and kill operation belongs to a non-production stage, hydrogen sulfide can be combusted, and hydrogen sulfide can not be separated and combusted in a normal production period; although the liquid desulfurizing agent has a wide application range, the liquid desulfurizing agent needs to be injected into equipment and places, increases the operation cost and cannot be added into a stratum, and the solid desulfurizing agent mainly comprises active iron oxide, zinc oxide and basic carbonate, is mainly used for gas desulfurization accumulated in a desulfurizing tower and desulfurizing in drilling fluid, does not have a slow release effect and needs to be continuously added, and is difficult to desulfurize with liquid in the process, so that an efficient and quick solution for desulfurizing is developed aiming at the hydrogen sulfide in the production process of a high-sulfur-content oil-gas well, the production efficiency is improved, and the production requirement of the sulfur-containing oil-gas well is met.
Chinese patent No. CN 102698576A, 10.3.2012 discloses a desulfurizing agent suitable for oil-gas well production, which comprises the following components in percentage by mass: 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 removal agent is mutually soluble with water, the hydrogen sulfide in crude oil or natural gas can be effectively reduced, the hydrogen sulfide content in the crude oil or the natural gas can be less than 2ppm, and meanwhile, the product generated by the sulfur removal agent and the hydrogen sulfide is dissolved in water, so that a shaft cannot be blocked and the normal production of an oil-gas well cannot be influenced; the sulfur removal agent can function at a temperature in the range of 30-120 ℃ and reacts rapidly with hydrogen sulfide. Chinese patent No. CN104629700A, 5.20.2015, discloses a sulfur removal agent for a water producing oil well and a water producing gas well, which consists of the following components in percentage by weight: 30-60% of one or a mixture of more than two of primary amine or secondary amine compounds, alcohol amine compounds and pyridine compounds and 5-20% of alcohol; finally, the water is filled to 100 percent. The desulfurizing agent is easy to obtain, nontoxic, reasonable in price, convenient to transport, simple in field construction and free of corrosion to oil and gas well production pipelines and instruments. And the sulfur removing agent is a liquid adsorption type sulfur removing agent, and can generate a neutralization chemical reaction with hydrogen sulfide in oil, gas and water, so that the hydrogen sulfide in the oil gas and the sewage in the production process can be quickly removed.
The sulfur removal agents represented by the above patents are mainly liquid sulfur removal agents, mainly alkanolamine and nitrogen-containing sulfur removal agents, and although the sulfur removal agents have good application effects, the sulfur removal agents all need injection equipment and addition operation, so that the operation cost is increased, the sulfur removal agents cannot be directly added into a stratum for slow release, and the problems of low absorption capacity and poor high temperature resistance exist. Aiming at sulfur-containing oil and gas wells, in order to increase the long-term effect of measures for reducing hydrogen sulfide by slow release in a stratum and achieve underground desulfurization of the oil and gas wells in the whole production process so as to reduce consumption of non-production time, a formula of a solid slow-release desulfurizing agent needs to be developed to meet the requirement of long-term desulfurization 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 time of dissolution and slow release of the solid desulfurizer can reach 200 days when the solid desulfurizer is used for desulfurization under stratum conditions, continuous addition is avoided, and additional injection equipment is not required, so that the cost is greatly reduced.
The purpose of the invention is realized by the following technical scheme:
a solid slow-release sulfur removal agent comprises the following components in percentage by weight:
a sulfur removal body: 50-70%;
adhesive agent: 1 to 5 percent;
reinforcing agent: 5 to 10 percent;
the balance of 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 polybutylene adipate-terephthalate, polyvinyl alcohol and polydioxanone.
A preparation method of a solid slow-release sulfur removal agent comprises the following steps:
step one, adding a sulfur removal body into a reactor, heating to 80 ℃, stirring the sulfur removal body for 20-30 min, adding a reinforcing agent, stirring for 20-30 min, adding a forming agent, stirring for 10-20 min, and finally adding an adhesive, and stirring for 30-40 min;
step two, heating the temperature of the reactor to 100 ℃, starting vacuumizing when the temperature is heated to 100 ℃, reacting for 30-40 min, then stopping heating the reactor, and reducing the temperature to 90-95 ℃ and keeping the temperature constant;
and step three, conveying the materials in the reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 90-95 ℃, and extruding and granulating by the double-screw extruder to obtain the solid slow-release sulfur removal agent.
Preferably, in the second step, the temperature rise speed is controlled to be 1-2 ℃/min during temperature rise.
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 by a screen to control the diameter and the length of the material.
Preferably, in the third step, the mixture is sieved by a sieve of 1-3 mm.
The beneficial effects of this technical scheme are as follows:
1. the solid slow-release sulfur removal agent provided by the invention has good slow-release performance. In the solid slow-release sulfur removal agent, the polybutylene adipate-terephthalate, the polyvinyl alcohol and the polydioxanone are slowly dissolved under the condition of formation water, and the hexamethylenetetramine, the trioxymethylene, the paraformaldehyde and the ethylene glycol dimethyl ether can be slowly released to provide reactive aldehyde groups, so that the hydrogen sulfide is removed, the slow release of the solid sulfur removal agent is facilitated, and the validity period is long. The time of dissolution and slow release of the solid desulfurizer can reach 200 days when the solid desulfurizer is used for desulfurization under stratum conditions, continuous addition is avoided, and additional injection equipment is not required, so that the cost is greatly reduced.
2. The solid slow-release desulfurizing agent provided by the invention has the advantages of controllable particle size and convenience in transportation. The solid slow-release sulfur removal agent can be processed into solid particles with different particle sizes according to process requirements, and compared with liquid, the solid slow-release sulfur removal agent is convenient to transport.
3. The solid slow-release desulfurizing agent provided by the invention has high compressive strength and is added compositely. The solid slow-release sulfur removal agent has higher compressive strength, can be carried into a stratum in the fracturing and acidizing processes, can be used as a diversion diverting agent in the fracturing and acidizing processes to improve the measure effect, and can also be used as a conventional solid sulfur removal agent.
4. The solid slow-release desulfurizing agent provided by the invention is suitable for removing hydrogen sulfide by gas or liquid. The solid slow-release sulfur removal agent can be used for gas desulfurization and liquid desulfurization.
5. The solid slow-release sulfur removal agent provided by the invention does not contain metal ions. The solid slow-release sulfur removal agent does not contain any metal ions such as calcium, magnesium, iron and the like, and does not form metal ion precipitates to pollute the stratum under the condition of no stratum.
6. The invention provides a solid slow-release desulfurizing agent, which is used for underground desulfurization. The solid slow-release desulfurizing agent can be used for desulfurizing under the stratum condition, and has the characteristics of high efficiency, long time and the like.
7. According to the preparation method of the solid slow-release desulfurizing agent provided by the invention, liquid and solid in the formula are fully mixed, so that conditions are created for subsequent granulation; vacuumizing to prevent bubbles from being mixed in the particles to influence the compression resistance and other performances of the product; the double-screw extruder can prepare the product into granular solid, and meets the requirements of the product on particle size and compression resistance.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
It will be understood that when an element is referred to as being "on," "secured to" 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 the terms of orientation such as left, right, up and down in the embodiments of the present invention are only relative to each other or are referred to the normal use state of the product, and should not be considered as limiting.
Example 1
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 70 percent of sulfur removal body; 5% of an adhesive; 8% of a reinforcing agent; the balance of forming agent.
Wherein: the sulfur removal body consists of 50 weight percent of hexamethylenetetramine, 25 weight percent of trioxymethylene and 25 weight percent of 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 enhancer consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylamino ethanol; the forming agent consists of 70 weight percent of polybutylene adipate-terephthalate, 15 weight percent of polyvinyl alcohol and 15 weight percent of polydioxanone.
A preparation method of a solid slow-release sulfur removal agent comprises the following steps:
adding a formula amount of sulfur removal body into an intermittent stirring reactor, heating to 80 ℃, adding the formula amount of sulfur removal body, stirring for 20 min, adding a formula amount of reinforcing agent, stirring for 20 min, adding a formula amount of forming agent, stirring for 10 min, adding a formula amount of adhesive, and stirring for 30 min;
step two, heating the temperature of the batch type 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, then stopping heating the batch type stirring reactor, controlling the cooling speed to be 0.5 ℃/min, reducing the temperature to 90 ℃ and keeping the temperature constant;
and step three, conveying the material in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 90 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 1-1.8 mm to control the diameter and the length of the material to obtain the solid slow-release sulfur removal agent.
Example 2
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 50% of sulfur removal body; 5% of adhesive; 10% of a reinforcing agent; the balance of 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 weight percent of paraformaldehyde and 30 weight percent of beta-cyclodextrin; the enhancer consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylamino ethanol; the forming agent consists of 70 weight percent of poly (butylene adipate-terephthalate), 15 weight percent of polyvinyl alcohol and 15 weight percent of poly (p-dioxanone).
A preparation method of a solid slow-release sulfur removal agent comprises the following steps:
step one, adding a formula amount of a body into an intermittent stirring reactor, heating to 80 ℃, adding the formula amount of the body, stirring for 25 min, adding a formula amount of a reinforcing agent, stirring for 25 min, adding a formula amount of a forming agent, stirring for 15 min, adding a formula amount of a bonding agent, and stirring for 35 min;
step two, heating the temperature of the batch type stirring reactor to 100 ℃, controlling the heating speed to be 1.5 ℃/min, starting vacuumizing (vacuumizing till 0.85 MPa) when the temperature is raised to 100 ℃, reacting for 35 min, then stopping heating the batch type stirring reactor, controlling the cooling speed to be 0.75 ℃/min, and reducing the temperature to 92.5 ℃ and keeping the temperature constant;
and step three, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 92.5 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 1.8-2.4mm to control the diameter and the length of the materials to obtain the solid slow-release sulfur removal agent.
Example 3
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 60% of sulfur removal body; 3% of adhesive; 5% of a reinforcing agent; the balance of forming agent.
Wherein: the sulfur removal body consists of 30 weight percent of hexamethylenetetramine, 57 weight percent of trioxymethylene and 13 weight percent of 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 forming agent consists of 70 weight percent of polybutylene adipate-terephthalate and 30 weight percent of polyvinyl alcohol.
A preparation method of a solid slow-release desulfurizing agent comprises the following steps:
step one, adding a formula amount of a body into an intermittent stirring reactor, heating to 80 ℃, adding the formula amount of the body, stirring for 30 min, adding a formula amount of a reinforcing agent, stirring for 30 min, adding a formula amount of a forming agent, stirring for 20 min, adding a formula amount of a bonding agent, and stirring for 40 min;
step two, heating the temperature of the batch type 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, then stopping heating the batch type stirring reactor, controlling the cooling speed to be 1 ℃/min, reducing the temperature to 95 ℃ and keeping the temperature constant;
and step three, conveying the material in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 95 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 2.4-3 mm to control the diameter and the length of the material to obtain the solid slow-release sulfur removal agent.
Example 4
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 55% of sulfur removal body; 3% of adhesive; 5% of a reinforcing agent; the balance of forming agent.
Wherein: the sulfur removal body consists of 80 weight percent of trioxymethylene and 20 weight percent of 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-methylamino ethanol; the forming agent consists of 70 percent of polybutylene adipate-terephthalate, 10 percent of polyvinyl alcohol and 20 percent of polydioxanone by weight percentage.
A preparation method of a solid slow-release sulfur removal agent comprises the following steps:
step one, adding a formula amount of a body into an intermittent stirring reactor, heating to 80 ℃, adding the formula amount of the body, stirring for 30 min, adding a formula amount of a reinforcing agent, stirring for 30 min, adding a formula amount of a forming agent, stirring for 20 min, adding a formula amount of a bonding agent, and stirring for 40 min;
step two, heating the temperature of the batch type stirring reactor to 100 ℃, controlling the heating speed to be 2 ℃/min, starting vacuumizing (vacuumizing till 0.8 MPa) when the temperature is raised to 100 ℃, reacting for 40 min, then stopping heating the batch type stirring reactor, controlling the cooling speed to be 1 ℃/min, reducing the temperature to 95 ℃ and keeping the temperature constant;
and step three, conveying the material in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 95 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 2.4-3 mm to control the diameter and the length of the material to obtain the solid slow-release sulfur removal agent.
Example 5
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 60% of sulfur removal body; 1% of adhesive; 8% of a reinforcing agent; the balance of forming agent.
Wherein: the sulfur removal body is composed of 100 weight percent of hexamethylenetetramine; the adhesive consists of 70 weight percent of paraformaldehyde and 30 weight percent of polyethylene glycol; the reinforcing agent consists of 2-methylamino ethanol; the forming agent consists of 70 percent of polybutylene adipate-terephthalate, 10 percent of polyvinyl alcohol and 20 percent of polydioxanone by weight percentage.
A preparation method of a solid slow-release sulfur removal agent comprises the following steps:
step one, adding a formula amount of a body into an intermittent stirring reactor, heating to 80 ℃, adding the formula amount of the body, stirring for 30 min, adding a formula amount of a reinforcing agent, stirring for 30 min, adding a formula amount of a forming agent, stirring for 20 min, adding a formula amount of a bonding agent, and stirring for 40 min;
step two, heating the temperature of the batch type 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, then stopping heating the batch type stirring reactor, controlling the cooling speed to be 1 ℃/min, reducing the temperature to 95 ℃ and keeping the temperature constant;
and step three, conveying the material in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 95 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 2.4-3 mm to control the diameter and the length of the material to obtain the solid slow-release sulfur removal agent.
Comparative example 1
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 75% of sulfur removal body; 5% of an adhesive; 8% of a reinforcing agent; the balance of forming agent.
Wherein: the sulfur removal body consists of 50 weight percent of hexamethylenetetramine, 25 weight percent of trioxymethylene and 25 weight percent of 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 enhancer consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylamino ethanol; the forming agent consists of 70 weight percent of polybutylene adipate-terephthalate, 15 weight percent of polyvinyl alcohol and 15 weight percent of polydioxanone.
A preparation method of a solid slow-release sulfur removal agent comprises the following steps:
adding a formula amount of sulfur removal body into an intermittent stirring reactor, heating to 80 ℃, adding the formula amount of sulfur removal body, stirring for 20 min, adding a formula amount of reinforcing agent, stirring for 20 min, adding a formula amount of forming agent, stirring for 10 min, adding a formula amount of adhesive, and stirring for 30 min;
step two, raising the temperature of the batch type stirring reactor to 100 ℃, controlling the temperature raising speed to be 1 ℃/min, starting vacuumizing (vacuumizing till 0.8 MPa) when the temperature is raised to 100 ℃, reacting for 30 min, then stopping heating the batch type stirring reactor, controlling the temperature lowering speed to be 0.5 ℃/min, reducing the temperature to 90 ℃ and keeping the temperature constant;
and step three, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 90 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 1-1.8 mm to control the diameter and the length of the materials to obtain the solid slow-release sulfur removal agent.
Comparative example 2
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 70% of sulfur removal body; 6% of adhesive; 8% of a reinforcing agent; the balance of forming agent.
Wherein: the sulfur removal body consists of 50 weight percent of hexamethylenetetramine, 25 weight percent of trioxymethylene and 25 weight percent of 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 enhancer consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylamino ethanol; the forming agent consists of 70 weight percent of poly (butylene adipate-terephthalate), 15 weight percent of polyvinyl alcohol and 15 weight percent of poly (p-dioxanone).
A preparation method of a solid slow-release sulfur removal agent comprises the following steps:
adding a formula amount of sulfur removal body into an intermittent stirring reactor, heating to 80 ℃, adding the formula amount of sulfur removal body, stirring for 20 min, adding a formula amount of reinforcing agent, stirring for 20 min, adding a formula amount of forming agent, stirring for 10 min, adding a formula amount of adhesive, and stirring for 30 min;
step two, raising the temperature of the batch type stirring reactor to 100 ℃, controlling the temperature raising speed to be 1 ℃/min, starting vacuumizing (vacuumizing till 0.8 MPa) when the temperature is raised to 100 ℃, reacting for 30 min, then stopping heating the batch type stirring reactor, controlling the temperature lowering speed to be 0.5 ℃/min, reducing the temperature to 90 ℃ and keeping the temperature constant;
and step three, conveying the material in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 90 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 1-1.8 mm to control the diameter and the length of the material to obtain the solid slow-release sulfur removal agent.
Comparative example 3
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 70 percent of sulfur removal body; 5% of adhesive; 12% of a reinforcing agent; the balance of forming agent.
Wherein: the sulfur removal body consists of 50 weight percent of hexamethylenetetramine, 25 weight percent of trioxymethylene and 25 weight percent of 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 enhancer consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylamino ethanol; the forming agent consists of 70 weight percent of polybutylene adipate-terephthalate, 15 weight percent of polyvinyl alcohol and 15 weight percent of polydioxanone.
A preparation method of a solid slow-release desulfurizing agent comprises the following steps:
adding a formula amount of sulfur removal body into an intermittent stirring reactor, heating to 80 ℃, adding the formula amount of sulfur removal body, stirring for 20 min, adding a formula amount of reinforcing agent, stirring for 20 min, adding a formula amount of forming agent, stirring for 10 min, adding a formula amount of adhesive, and stirring for 30 min;
step two, heating the temperature of the batch type 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, then stopping heating the batch type stirring reactor, controlling the cooling speed to be 0.5 ℃/min, reducing the temperature to 90 ℃ and keeping the temperature constant;
and step three, conveying the material in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 90 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 1-1.8 mm to control the diameter and the length of the material to obtain the solid slow-release sulfur removal agent.
Comparative example 4
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 45% of sulfur removal body; 5% of adhesive; 10% of a reinforcing agent; the balance of 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 weight percent of paraformaldehyde and 30 weight percent of beta-cyclodextrin; the enhancer consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylamino ethanol; the forming agent consists of 70 weight percent of polybutylene adipate-terephthalate, 15 weight percent of polyvinyl alcohol and 15 weight percent of polydioxanone.
A preparation method of a solid slow-release sulfur removal agent comprises the following steps:
step one, adding a formula amount of a body into an intermittent stirring reactor, heating to 80 ℃, adding the formula amount of the body, stirring for 25 min, adding a formula amount of a reinforcing agent, stirring for 25 min, adding a formula amount of a forming agent, stirring for 15 min, adding a formula amount of a bonding agent, and stirring for 35 min;
step two, heating the temperature of the batch type stirring reactor to 100 ℃, controlling the heating speed to be 1.5 ℃/min, starting vacuumizing (vacuumizing till 0.85 MPa) when the temperature is raised to 100 ℃, reacting for 35 min, then stopping heating the batch type stirring reactor, controlling the cooling speed to be 0.75 ℃/min, and reducing the temperature to 92.5 ℃ and keeping the temperature constant;
and step three, conveying the material in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 92.5 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 1.8-2.4mm to control the diameter and the length of the material, thereby obtaining the solid slow-release sulfur removal agent.
Comparative example 5
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 50% of sulfur removal body; 0.5% of adhesive; 10% of a reinforcing agent; the balance of 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 weight percent of paraformaldehyde and 30 weight percent of beta-cyclodextrin; the enhancer consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylamino ethanol; the forming agent consists of 70 weight percent of poly (butylene adipate-terephthalate), 15 weight percent of polyvinyl alcohol and 15 weight percent of poly (p-dioxanone).
A preparation method of a solid slow-release desulfurizing agent comprises the following steps:
step one, adding a formula amount of a body into an intermittent stirring reactor, heating to 80 ℃, adding the formula amount of the body, stirring for 25 min, adding a formula amount of a reinforcing agent, stirring for 25 min, adding a formula amount of a forming agent, stirring for 15 min, adding a formula amount of a bonding agent, and stirring for 35 min;
step two, heating the temperature of the batch type stirring reactor to 100 ℃, controlling the heating speed to be 1.5 ℃/min, starting vacuumizing (vacuumizing till 0.85 MPa) when the temperature is raised to 100 ℃, reacting for 35 min, then stopping heating the batch type stirring reactor, controlling the cooling speed to be 0.75 ℃/min, and reducing the temperature to 92.5 ℃ and keeping the temperature constant;
and step three, conveying the material in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 92.5 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 1.8-2.4mm to control the diameter and the length of the material, thereby obtaining the solid slow-release sulfur removal agent.
Comparative example 6
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 50% of sulfur removal body; 5% of an adhesive; 4% of a reinforcing agent; the balance of 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 weight percent of paraformaldehyde and 30 weight percent of beta-cyclodextrin; the enhancer consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylamino ethanol; the forming agent consists of 70 weight percent of poly (butylene adipate-terephthalate), 15 weight percent of polyvinyl alcohol and 15 weight percent of poly (p-dioxanone).
A preparation method of a solid slow-release sulfur removal agent comprises the following steps:
step one, adding a formula amount of a body into an intermittent stirring reactor, heating to 80 ℃, adding the formula amount of the body, stirring for 25 min, adding a formula amount of a reinforcing agent, stirring for 25 min, adding a formula amount of a forming agent, stirring for 15 min, adding a formula amount of a bonding agent, and stirring for 35 min;
step two, heating the temperature of the batch type stirring reactor to 100 ℃, controlling the heating speed to be 1.5 ℃/min, starting vacuumizing (vacuumizing till 0.85 MPa) when the temperature is raised to 100 ℃, reacting for 35 min, then stopping heating the batch type stirring reactor, controlling the cooling speed to be 0.75 ℃/min, and reducing the temperature to 92.5 ℃ and keeping the temperature constant;
and step three, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 92.5 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 1.8-2.4mm to control the diameter and the length of the materials to obtain the solid slow-release sulfur removal agent.
Comparative example 7
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 60% of sulfur removal body; 3% of adhesive; 5% of a reinforcing agent; the balance of forming agent.
Wherein: the sulfur removal body consists of 30 weight percent of hexamethylenetetramine, 57 weight percent of trioxymethylene and 13 weight percent of 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 forming agent consists of 70 weight percent of polybutylene adipate-terephthalate and 30 weight percent of polyvinyl alcohol.
A preparation method of a solid slow-release desulfurizing agent comprises the following steps:
step one, adding a formula amount of a body into an intermittent stirring reactor, heating to 75 ℃, adding the formula amount of the body, stirring for 30 min, adding a formula amount of a reinforcing agent, stirring for 30 min, adding a formula amount of a forming agent, stirring for 20 min, adding a formula amount of a bonding agent, and stirring for 40 min;
step two, heating the temperature of the batch type stirring reactor to 100 ℃, controlling the heating speed to be 2 ℃/min, starting vacuumizing (vacuumizing till 0.9 MPa) when the temperature is raised to 100 ℃, reacting for 40 min, then stopping heating the batch type stirring reactor, controlling the cooling speed to be 1 ℃/min, reducing the temperature to 95 ℃ and keeping the temperature constant;
and step three, conveying the material in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 95 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 2.4-3 mm to control the diameter and the length of the material to obtain the solid slow-release sulfur removal agent.
Comparative example 8
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 60% of sulfur removal body; 3% of adhesive; 5% of a reinforcing agent; the balance of forming agent.
Wherein: the sulfur removal body consists of 30 weight percent of hexamethylenetetramine, 57 weight percent of trioxymethylene and 13 weight percent of 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 forming agent consists of 70 weight percent of polybutylene adipate-terephthalate and 30 weight percent of polyvinyl alcohol.
A preparation method of a solid slow-release sulfur removal agent comprises the following steps:
step one, adding a formula amount of a body into an intermittent stirring reactor, heating to 85 ℃, adding the formula amount of the body, stirring for 30 min, adding a formula amount of a reinforcing agent, stirring for 30 min, adding a formula amount of a forming agent, stirring for 20 min, adding a formula amount of a bonding agent, and stirring for 40 min;
step two, heating the temperature of the batch type stirring reactor to 100 ℃, controlling the heating speed to be 2 ℃/min, starting vacuumizing (vacuumizing till 0.9 MPa) when the temperature is raised to 100 ℃, reacting for 40 min, then stopping heating the batch type stirring reactor, controlling the cooling speed to be 1 ℃/min, reducing the temperature to 95 ℃ and keeping the temperature constant;
and step three, conveying the material in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 95 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 2.4-3 mm to control the diameter and the length of the material to obtain the solid slow-release sulfur removal agent.
Comparative example 9
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 55% of sulfur removal body; 3% of adhesive; 5% of a reinforcing agent; the balance of forming agent.
Wherein: the sulfur removal body consists of 80 weight percent of trioxymethylene and 20 weight percent of 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-methylamino ethanol; the forming agent consists of 70 percent of polybutylene adipate-terephthalate, 10 percent of polyvinyl alcohol and 20 percent of polydioxanone by weight percentage.
A preparation method of a solid slow-release sulfur removal agent comprises the following steps:
step one, adding a formula amount of a body into an intermittent stirring reactor, heating to 80 ℃, adding the formula amount of the body, stirring for 30 min, adding a formula amount of a reinforcing agent, stirring for 30 min, adding a formula amount of a forming agent, stirring for 20 min, adding a formula amount of a bonding agent, and stirring for 40 min;
step two, heating the temperature of the batch type stirring reactor to 95 ℃, controlling the heating speed to be 2 ℃/min, starting vacuumizing (vacuumizing to 0.8 MPa) when the temperature is raised to 95 ℃, reacting for 40 min, then stopping heating the batch type stirring reactor, controlling the cooling speed to be 1 ℃/min, reducing the temperature to 85 ℃ and keeping the temperature constant;
and step three, conveying the material in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 85 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 2.4-3 mm to control the diameter and the length of the material to obtain the solid slow-release sulfur removal agent.
Comparative example 10
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 55% of sulfur removal body; 3% of adhesive; 5% of a reinforcing agent; the balance of forming agent.
Wherein: the sulfur removal body consists of 80 weight percent of trioxymethylene and 20 weight percent of 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-methylamino ethanol; the forming agent consists of 70 weight percent of polybutylene adipate-terephthalate, 10 weight percent of polyvinyl alcohol and 20 weight percent of polydioxanone.
A preparation method of a solid slow-release desulfurizing agent comprises the following steps:
step one, adding a formula amount of a body into an intermittent stirring reactor, heating to 110 ℃, adding the formula amount of the body, stirring for 30 min, adding a formula amount of a reinforcing agent, stirring for 30 min, adding a formula amount of a forming agent, stirring for 20 min, adding a formula amount of a bonding agent, and stirring for 40 min;
step two, heating the temperature of the batch type stirring reactor to 100 ℃, controlling the heating speed to be 2 ℃/min, starting vacuumizing (vacuumizing till 0.8 MPa) when the temperature is raised to 100 ℃, reacting for 40 min, then stopping heating the batch type stirring reactor, controlling the cooling speed to be 1 ℃/min, reducing the temperature to 85 ℃ and keeping the temperature constant;
and step three, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 100 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 2.4-3 mm to control the diameter and the length of the materials to obtain the solid slow-release sulfur removal agent.
Comparative example 11
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 60% of sulfur removal body; 1% of adhesive; 8% of a reinforcing agent; the rest is forming agent.
Wherein: the sulfur removal body is composed of 100 weight percent of hexamethylenetetramine; the adhesive consists of 70 weight percent of paraformaldehyde and 30 weight percent of polyethylene glycol; the reinforcing agent consists of 2-methylamino ethanol; the forming agent consists of 70 weight percent of polybutylene adipate-terephthalate, 10 weight percent of polyvinyl alcohol and 20 weight percent of polydioxanone.
A preparation method of a solid slow-release sulfur removal agent comprises the following steps:
step one, adding a formula amount of a body into an intermittent stirring reactor, heating to 80 ℃, adding the formula amount of the body, stirring for 30 min, adding a formula amount of a reinforcing agent, stirring for 30 min, adding a formula amount of a forming agent, stirring for 20 min, adding a formula amount of a bonding agent, and stirring for 40 min;
step two, heating the temperature of the batch type 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, then stopping heating the batch type stirring reactor, controlling the cooling speed to be 1.5 ℃/min, and reducing the temperature to 95 ℃ and keeping the temperature constant;
and step three, conveying the materials in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 95 ℃, extruding and granulating by the double-screw extruder, and sieving by a screen of 2.4-3 mm to control the diameter and the length of the materials to obtain the solid slow-release sulfur removal agent.
Comparative example 12
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 60% of sulfur removal body; 1% of adhesive; 8% of a reinforcing agent; the balance of forming agent.
Wherein: the sulfur removal body is composed of 100 weight percent of hexamethylenetetramine; the adhesive consists of 70 weight percent of paraformaldehyde and 30 weight percent of polyethylene glycol; the reinforcing agent consists of 2-methylamino ethanol; the forming agent consists of 70 weight percent of polybutylene adipate-terephthalate, 10 weight percent of polyvinyl alcohol and 20 weight percent of polydioxanone.
A preparation method of a solid slow-release sulfur removal agent comprises the following steps:
step one, adding a formula amount of a body into an intermittent stirring reactor, heating to 80 ℃, adding the formula amount of the body, stirring for 30 min, adding a formula amount of a reinforcing agent, stirring for 30 min, adding a formula amount of a forming agent, stirring for 20 min, adding a formula amount of a bonding agent, and stirring for 40 min;
step two, heating the temperature of the batch type stirring reactor to 100 ℃, controlling the heating speed to be 0.5 ℃/min, starting vacuumizing (vacuumizing till 0.9 MPa) when the temperature is raised to 100 ℃, reacting for 40 min, then stopping heating the batch type stirring reactor, controlling the cooling speed to be 0.25 ℃/min, and reducing the temperature to 95 ℃ and keeping constant;
and step three, conveying the material in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 95 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 2.4-3 mm to control the diameter and the length of the material to obtain the solid slow-release sulfur removal agent.
Comparative example 13
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 70% of sulfur removal body; 5% of adhesive; 8% of a reinforcing agent; the rest is forming agent.
Wherein: the sulfur removal body consists of 50 weight percent of hexamethylenetetramine, 25 weight percent of trioxymethylene and 25 weight percent of 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 enhancer consists of 20 weight percent of diglycolamine and 80 weight percent of 2-methylamino ethanol; the forming agent consists of 70 weight percent of polybutylene adipate-terephthalate, 15 weight percent of polyvinyl alcohol and 15 weight percent of polydioxanone.
A preparation method of a solid slow-release sulfur removal agent comprises the following steps:
adding a formula amount of sulfur removal body into an intermittent stirring reactor, heating to 80 ℃, adding the formula amount of sulfur removal body, stirring for 20 min, adding a formula amount of reinforcing agent, stirring for 20 min, adding a formula amount of forming agent, stirring for 10 min, adding a formula amount of adhesive, and stirring for 30 min;
step two, raising the temperature of the batch type stirring reactor to 100 ℃, controlling the temperature raising speed to be 1 ℃/min, starting vacuumizing (vacuumizing till 0.75 MPa) when the temperature is raised to 100 ℃, reacting for 30 min, then stopping heating the batch type stirring reactor, controlling the temperature lowering speed to be 0.5 ℃/min, reducing the temperature to 90 ℃ and keeping the temperature constant;
and step three, conveying the material in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 90 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 1-1.8 mm to control the diameter and the length of the material to obtain the solid slow-release sulfur removal agent.
Comparative example 14
The invention discloses a solid slow-release desulfurizing agent, which comprises the following components in percentage by weight: 70% of sulfur removal body; 5% of an adhesive; 8% of a reinforcing agent; the balance of forming agent.
Wherein: the sulfur removal body consists of 50 weight percent of hexamethylenetetramine, 25 weight percent of trioxymethylene and 25 weight percent of 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 enhancer is composed of 20 wt% of diglycolamine, 80 wt% of 2-methylaminoethanol; the forming agent consists of 70 weight percent of polybutylene adipate-terephthalate, 15 weight percent of polyvinyl alcohol and 15 weight percent of polydioxanone.
A preparation method of a solid slow-release desulfurizing agent comprises the following steps:
adding a formula amount of sulfur removal body into an intermittent stirring reactor, heating to 80 ℃, adding the formula amount of sulfur removal body, stirring for 20 min, adding a formula amount of reinforcing agent, stirring for 20 min, adding a formula amount of forming agent, stirring for 10 min, adding a formula amount of adhesive, and stirring for 30 min;
step two, raising the temperature of the batch type stirring reactor to 100 ℃, controlling the temperature raising speed to be 1 ℃/min, starting vacuumizing (vacuumizing till 0.95 MPa) when the temperature is raised to 100 ℃, reacting for 30 min, then stopping heating the batch type stirring reactor, controlling the temperature lowering speed to be 0.5 ℃/min, reducing the temperature to 90 ℃ and keeping the temperature constant;
and step three, conveying the material in the stirring reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 90 ℃, extruding and granulating by the double-screw extruder, and sieving by a sieve of 1-1.8 mm to control the diameter and the length of the material to obtain the solid slow-release sulfur removal agent.
The solid slow-release sulfur removal agents obtained in examples 1 to 5 and comparative examples 1 to 14 were subjected to a water dissolution test, a hydrogen sulfide absorption performance test and a pressure-bearing test at different temperatures.
1. And (4) dissolution testing.
Taking 1 g solid slow-release sulfur removal agent (the particle size range is 1-3 mm), placing the solid slow-release sulfur removal agent in a test tube with a plug, pouring 100 mL distilled water, placing the test tube in a water bath kettle at 65 ℃, filtering after 24 hours, adding the solid on the filter paper into 100 ml of distilled water again, continuously measuring the dissolved amount in different time periods, repeating the steps, and calculating the dissolving rate.
2. Test of Hydrogen sulfide absorption Performance
The 1.0 mL hydrochloric acid solution was removed, placed in a 15 mL plastic tube, and transferred to a 500 mL anaerobic bottle. Adding 0.5 mL sodium sulfide solution into plastic test tube, and quickly covering anaerobic bottleStopper, shake body for 10 weeks, put in oven at 60 deg.C, shake body every 5 min for 10 weeks. 20 After min, the filtrates in the dissolution test were poured into the bottom of an anaerobic bottle at different time periods, the body was shaken for 10 weeks, and the bottle was placed in an oven at 60 ℃.30 Detecting H in bottle by using gas detection hand pump and hydrogen sulfide detection tube after min 2 S gas content is read, and simultaneously, a blank experiment is carried out, wherein a gas detection hand pump and a hydrogen sulfide detection tube are used for detecting H in a bottle in the blank experiment 2 S gas content and reading. After the experiment, the anaerobic bottle is placed in a fume hood, and excess sodium hydroxide solution is used for absorbing residual hydrogen sulfide gas. 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
In the formula: x-desulfurization Rate,% (desulfurizing time 5 min)
C1-Hydrogen sulfide content in blank test, ppm
C2 Determination of the Hydrogen sulfide content in the experiment, ppm
3. And (6) carrying out pressure bearing test.
Taking the solid slow-release sulfur removal agent (the particle size range is 1-3 mm), carrying out a breakage rate test in a press, wherein the breakage rate is extremely low when the pressure is within 10 MPa, the average breakage rate is about 3%, and the compressive capacity is measured under the condition of 10% breakage rate.
The qualified product has a dissolution rate (%) of 10 d: 0.05-0.15, 100d dissolution (%): 45-50, the dissolution rate (%) at 200d is 96-100, and the sulfur removal rate (%) at 10d is more than or equal to 98; the sulfur removal rate (%) is more than or equal to 99 at 100 d; 200d sulfur removal rate (%) =100; the bearing pressure (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 performance, liquid carrying capacity, and scale inhibition rate, and the data are shown in the following table:
through the tests of examples 1-5 and comparative examples 1-14, it can be known that the composition and the proportion of a sulfur removal body, a bonding agent, a reinforcing agent and a forming agent are required to be specified, and the qualified solid slow-release sulfur removal agent can be obtained only by the specific preparation steps and process parameters.
The above 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 modifications and equivalent variations of the above embodiment according to the technical spirit of the present invention are within the scope of the present invention.
Claims (10)
1. The solid slow-release sulfur removal agent is characterized by comprising the following components in percentage by weight:
a sulfur removal body: 50-70%;
adhesive agent: 1 to 5 percent;
reinforcing agent: 5 to 10 percent;
the balance of forming agent.
2. The solid slow-release sulfur removal agent of claim 1, which is characterized in that: the sulfur removal body is one or more of hexamethylenetetramine, trioxymethylene and ethylene glycol dimethyl ether.
3. The solid slow-release sulfur removal agent of claim 2, which is characterized in that: the adhesive is two or three of paraformaldehyde, beta-cyclodextrin and polyethylene glycol.
4. The solid slow-release sulfur removal agent according to claim 3, wherein: the reinforcing agent is one or more of diglycolamine and 2-methylamino ethanol.
5. The solid slow-release sulfur removal agent according to claim 4, wherein: the forming agent is one or more of polybutylene adipate-terephthalate, polyvinyl alcohol and polydioxanone.
6. The preparation method of the solid slow-release desulfurizing agent is characterized by comprising the following steps:
step one, adding a sulfur removal body into a reactor, heating to 80 ℃, stirring the sulfur removal body for 20-30 min, adding a reinforcing agent, stirring for 20-30 min, adding a forming agent, stirring for 10-20 min, and finally adding an adhesive, and stirring for 30-40 min;
step two, heating the temperature of the reactor to 100 ℃, starting vacuumizing when the temperature is heated to 100 ℃, reacting for 30-40 min, then stopping heating the reactor, and reducing the temperature to 90-95 ℃ and keeping the temperature constant;
and step three, conveying the materials in the reactor to a double-screw extruder, controlling the temperature of the double-screw extruder at 90-95 ℃, and extruding and granulating by the double-screw extruder to obtain the solid slow-release sulfur removal agent.
7. The preparation method of the solid slow-release sulfur removal agent according to claim 6, characterized in that: in the second step, the temperature rising speed is controlled to be 1-2 ℃/min during temperature rising.
8. The preparation method of the solid slow-release sulfur removal agent according to claim 7, characterized in that: and in the second step, vacuumizing until the pressure is between 0.8 and 0.9 MPa.
9. The preparation method of the solid slow-release sulfur removal agent according to claim 8, characterized in that: in the second step, the cooling speed is controlled to be 0.5-1.0 ℃/min during cooling.
10. The preparation method of the solid slow-release sulfur removal agent according to claim 9, characterized in that: in the third step, the solid slow-release sulfur removing agent is screened by a 1-3 mm screen to control the diameter and the length of the material.
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