CN111330545B - High-efficiency desulfurizer with indication function and preparation method thereof - Google Patents
High-efficiency desulfurizer with indication function and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of hydrogen sulfide treatment, and particularly discloses a high-efficiency desulfurizer with an indication function and a preparation method thereof. The desulfurizer comprises the following components in parts by weight: 10-60 parts of alkaline compound, 20-50 parts of basic copper carbonate, 10-30 parts of nano powder and 0-25 parts of surface modifier, wherein the alkaline compound does not comprise the basic copper carbonate; and/or the desulfurizing agent comprises the following components in parts by weight: 30-110 parts of basic copper carbonate, 10-30 parts of nano powder and 0-25 parts of surface modifier; the modified diatomite floor also comprises 5-10 parts of activated carbon, 5-10 parts of diatomite, 2-8 parts of a hydrophobic agent and 2-10 parts of a dispersing agent. The invention provides a high-efficiency desulfurizer with an indication function, which is characterized in that desulfurizer powder with a large specific surface area is prepared by adopting a nanotechnology, so that the desulfurizer powder can react with hydrogen sulfide more thoroughly, the absorption efficiency is higher, the final dosage of the desulfurizer can be controlled by adding an indicator, the dosage can be controlled, and the problem that whether hydrogen sulfide is completely removed or not cannot be judged is solved.
Description
Technical Field
The invention relates to the technical field of hydrogen sulfide treatment, in particular to a high-efficiency desulfurizer with an indication function and a preparation method thereof.
Background
Hydrogen sulfide (H)2S) is a highly toxic, colorless and transparent gas, heavier than air, and low-concentration hydrogen sulfide has a smell similar to that of a smelly egg; the olfactory nerve is paralyzed quickly at high content, no smell is produced, and the olfactory nerve is difficult to detect, and the inhalation of a small amount of high-concentration hydrogen sulfide can kill the olfactory nerve in a short time. When the content of hydrogen sulfide in the air exceeds 1.5 ppm, death of people can be caused. The hydrogen sulfide is commonly present in the industries of mining, metal smelting, exploitation and extraction of sulfur-containing petroleum and natural gas, rubber, leather making and the like. The death rate of hydrogen sulfide poisoning is high, accidents are sudden and group, personnel safety is seriously threatened once leakage accidents occur, secondary disasters have large influence, nearby air is seriously polluted, and the ecological environment is damaged.
With the large-scale production of high-content oil and gas fields and the increasing processing amount of high-sulfur crude oil, hydrogen sulfide has penetrated every corner of the petrochemical industry. At present, domestic research on hydrogen sulfide removal mainly focuses on industrial desulfurization, and methods such as water spraying, forced air dispersion, alkali liquor absorption and the like are mainly adopted for dealing with leakage of hydrogen sulfide gas. The water spray can generate a large amount of waste water containing hydrogen sulfide, and the threat of hydrogen sulfide can still exist by forced wind dispersion.
In recent years, research on sulfur removal agents, desulfurizing agents or hydrogen sulfide scavengers has been conducted, in which an alkaline compound (such as zinc carbonate, copper sulfate, potassium permanganate, sodium carbonate, sodium silicate, zinc oxide, iron oxide, etc.) and hydrogen sulfide are subjected to precipitation reaction and physical adsorption to convert hydrogen sulfide into a stable inert substance. However, the above-mentioned alkaline substance has problems of low desulfurization efficiency and poor absorption effect, and further has problems such as: zinc carbonate will regenerate hydrogen sulfide at lower pH; iron oxide is pulverized when meeting water, and carbon deposition reaction is carried out at a higher temperature in a reducing atmosphere; the copper sulfate reacts with hydrogen sulfide to generate sulfuric acid, which is easy to cause secondary damage; potassium permanganate is a strong oxidant, can cause secondary damage to the environment, and produces water after the reaction, and the waste is difficult to clean. In addition, the existing desulfurizer has the defect that whether hydrogen sulfide is completely removed cannot be judged, if the desulfurizer is used excessively, waste is easily caused, and if the hydrogen sulfide is not completely removed, equipment and personnel are easily damaged.
Disclosure of Invention
In view of the above disadvantages of the prior art, the present invention aims to provide a high efficiency desulfurizer with indication function and a preparation method thereof, which are used to solve the problems of low desulfurization efficiency, poor absorption effect, incapability of determining whether to completely remove hydrogen sulfide, and the like of the desulfurizer in the prior art.
In order to achieve the above objects and other related objects, in one aspect, the present invention provides a high efficiency desulfurizing agent with indication function, wherein the desulfurizing agent comprises the following components in parts by weight: 10-60 parts of alkaline compound, 20-50 parts of basic copper carbonate, 10-30 parts of nano powder and 0-25 parts of surface modifier, wherein the alkaline compound does not comprise the basic copper carbonate; and/or the desulfurizing agent comprises the following components in parts by weight: 30-110 parts of basic copper carbonate, 10-30 parts of nano powder and 0-25 parts of surface modifier.
Optionally, the desulfurizing agent further comprises the following components in parts by weight: 5-10 parts of activated carbon and 5-10 parts of diatomite.
Optionally, the alkaline compound is selected from at least one of zinc carbonate, basic zinc carbonate, sodium silicate, potassium hydroxide, sodium hydroxide, calcium hydroxide.
Optionally, the nanopowder is selected from at least one of nano-magnesia, nano-zinc oxide, nano-alumina and nano-titania.
Optionally, the surface modifier is selected from at least one of amino silicone oil, silane coupling agent HD110, silane coupling agent KH550, silane coupling agent KH570, water-soluble silicone oil, acetone and ethanol.
Optionally, the nanopowder has a particle size of 100-300 nanometers.
Optionally, the desulfurizing agent further comprises the following components in parts by weight: 2-8 parts of a hydrophobic agent and 2-10 parts of a dispersing agent.
Optionally, the hydrophobic agent is selected from at least one of potassium methyl silicate and fumed silica.
Optionally, the dispersant is selected from at least one of polycarboxylate dispersants, alkyl naphthalene sulfonates, sodium polyacrylates.
Optionally, the desulfurizing agent is a powdery solid with a particle size of 100-1500 nm, preferably 500-1000 nm.
Optionally, the pH of the saturated solution of the desulfurizing agent is more than or equal to 11, preferably 12.
In another aspect, the invention provides a preparation method of the high efficiency desulfurizing agent with the indicating function, which comprises the following steps:
(1) adding an alkaline compound and basic copper carbonate into water, and stirring and dispersing to obtain an alkaline compound dispersion system; dissolving the nano powder in water, adding part of surface modifier, stirring uniformly, and then performing ultrasonic dispersion to obtain a nano powder dispersion system;
(2) sequentially adding the alkaline compound dispersion system and the nano powder dispersion system obtained in the step (1) into water, uniformly stirring, finally adding the rest surface modifier, stirring and reacting to be viscous, and finally drying, cooling and grinding to obtain the desulfurizer;
wherein, when the desulfurizing agent also comprises a hydrophobic agent and/or a dispersant, the hydrophobic agent and/or the dispersant is added into the alkaline compound dispersion system in the step (1); when the desulfurizer also comprises activated carbon and/or diatomite, in the step (2), after the alkaline compound dispersion system and the nano powder dispersion system are uniformly stirred, the activated carbon and/or diatomite are sequentially added, and after uniform stirring, the surface modifier is added.
Optionally, in the step (1), the initial temperature of water for dispersing the basic compound is 10-30 ℃, the initial temperature of water for dispersing the nano powder is 50-60 ℃, and the temperature of water for ultrasonic dispersion is 50-70 ℃.
Optionally, in the step (1), the time for ultrasonic dispersion is 1-2 hours.
Optionally, in the step (2), the stirring temperature of the alkali compound dispersion system and the nano powder dispersion system is 10-90 ℃, and the stirring time is 30-90 min.
Optionally, in the step (2), the drying temperature is 80-110 ℃, and the drying time is 5-24 hours.
Optionally, the desulfurizing agent obtained in the step (2) is crushed into powder with the particle size of 100-1500 nanometers.
As mentioned above, the high-efficiency desulfurizer with indication function and the preparation method thereof of the invention have the following beneficial effects:
after a certain amount of basic copper carbonate is added into the formula of the desulfurizer, a black substance (copper sulfide) can be generated after the reaction of the desulfurizer and hydrogen sulfide and can be used as an indicator to judge whether the hydrogen sulfide is completely removed; the formula adopts the nano powder, and the specific surface area of the nano powder is increased after the nano powder is subjected to ultrasonic dispersion treatment, so that the reaction efficiency of the desulfurizer and the hydrogen sulfide can be effectively improved, and the absorption effect is improved; the diatomite and the active carbon are added into the formula, so that the absorption treatment rate of the hydrogen sulfide can be greatly improved; the hydrophobic agent can effectively improve the defect that alkaline compounds (such as basic zinc carbonate and the like) are easy to absorb water; in addition, the addition of the dispersing agent is beneficial to promoting the adjustment of the pH value of the alkaline compound and improving the suspension effect of the final finished product in the air.
In conclusion, the invention provides the high-efficiency desulfurizer with the indication function, the desulfurizer powder with larger specific surface area is prepared by adopting the nanotechnology, so that the desulfurizer powder can react with hydrogen sulfide more thoroughly, the absorption efficiency is higher, the final dosage of the desulfurizer can be controlled by adding the indicator, the dosage can be controlled, and the problems of low desulfurization efficiency, poor absorption effect and incapability of judging whether to be thoroughly removed in the prior art are solved.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
The invention provides a first high-efficiency desulfurizer with an indicating function, which comprises the following components in parts by weight: 10-60 parts of alkaline compound, 20-50 parts of basic copper carbonate, 10-30 parts of nano powder and 0-25 parts of surface modifier, wherein the alkaline compound does not comprise the basic copper carbonate.
The invention provides a second high-efficiency desulfurizer with an indicating function, which comprises the following components in parts by weight: 30-110 parts of basic copper carbonate, 10-30 parts of nano powder and 0-25 parts of surface modifier.
Further, the two desulfurizing agents also comprise the following components in parts by weight: 5-10 parts of activated carbon, 5-10 parts of diatomite, 2-8 parts of a hydrophobing agent and 2-10 parts of a dispersing agent.
Wherein the alkaline compound is at least one selected from zinc carbonate, basic zinc carbonate, sodium silicate, potassium hydroxide, sodium hydroxide and calcium hydroxide.
Wherein the nano powder is selected from at least one of nano magnesium oxide, nano zinc oxide, nano aluminum oxide and nano titanium dioxide. The particle size of the nano-powder is 100-300 nm, the particle size of the nano-magnesium oxide and the nano-zinc oxide used in the following examples is 100 nm, the particle size of the nano-aluminum oxide is 300 nm, and the particle size of the nano-titanium dioxide is 200 nm.
Wherein the surface modifier is selected from at least one of amino silicone oil, a silane coupling agent HD110, a silane coupling agent KH550, a silane coupling agent KH570, water-soluble silicone oil, acetone and ethanol; when the surface modifier is at least one selected from amino silicone oil, silane coupling agent HD110, silane coupling agent KH550, silane coupling agent KH570 and water-soluble silicone oil, the prepared desulfurizer contains 5-25 parts of surface modifier; when the surface modifier is at least one of acetone and ethanol, the propanol and the ethanol can volatilize in the drying process, and the prepared desulfurizer does not contain the surface modifier. KH550 is selected as the silane coupling agent in the following examples, and the effects of the other two silane coupling agents HD110 and KH570 are the same as KH 550. In the invention, the surface modifier has the main functions of modifying the surface of inorganic powder, coupling inorganic components such as nano powder, activated carbon and the like to form an inorganic/inorganic composite material, realizing surface modification and improving the adsorption capacity of the desulfurizer on hydrogen sulfide; and secondly, the dispersion aid is used for improving the dispersibility of the inorganic powder in a solvent, promoting the inorganic solid powder which is difficult to dissolve in water, particularly nano powder to stably and uniformly suspend and disperse in water, shortening the dispersion time, preventing solid powder particles from settling and agglomerating, and further promoting the coupling reaction between inorganic components.
Wherein the hydrophobic agent is at least one selected from potassium methyl silicate and gas phase silicon dioxide.
Wherein the dispersant is at least one selected from polycarboxylate dispersant, alkyl naphthalene sulfonate and sodium polyacrylate.
The preparation method of the desulfurizing agent comprises the following steps:
(1) adding an alkaline compound and basic copper carbonate into water with the initial temperature of 10-30 ℃, adding a dispersing agent and a hydrophobic agent, and uniformly stirring to obtain an alkaline compound dispersion system for later use; adding the nano powder into water with the initial temperature of 50-60 ℃, adding a proper amount of surface modifier, stirring for 1-2 hours, and ultrasonically dispersing for 1-2 hours at the temperature of 50-70 ℃ to obtain a nano powder dispersion system for later use.
(2) And (2) sequentially adding the alkaline compound dispersion system and the nano powder dispersion system obtained in the step (1) into water, mixing and stirring at 10-90 ℃ for 30-90min, sequentially adding active carbon and diatomite, continuously stirring for 60-90min, finally adding the rest surface modifier, stirring and reacting at 50-70 ℃ to be viscous, drying at 80-110 ℃ for 5-24 h, and cooling to room temperature to obtain the desulfurizer.
(3) The desulfurizer is crushed and ground into powder with the granularity of 100-1500 nanometers by a crusher.
The use method of the desulfurizer in the invention comprises the following steps:
the desulfurizer powder can be sprayed in the environment with hydrogen sulfide leakage by using a spraying device (the structural principle of the spraying device is similar to that of a dry powder fire extinguisher), and can also be directly sprayed in the environment with hydrogen sulfide leakage, and the use effect of the desulfurizer powder is better.
The desulfurizing agent is prepared according to the method, and the specific implementation process is as follows:
example 1
A high-efficiency desulfurizer with an indicating function comprises the following components in parts by weight:
20 parts of basic zinc carbonate, 20 parts of basic copper carbonate, 20 parts of nano titanium dioxide and 20 parts of a silane coupling agent KH 55020.
The preparation method of the desulfurizer comprises the following steps:
(1) adding basic zinc carbonate and basic copper carbonate into water with the initial temperature of 20 ℃, and uniformly stirring to obtain an alkaline compound dispersion system for later use; adding nano titanium dioxide into water with the initial temperature of 60 ℃, adding 2 parts of silane coupling agent KH550, stirring for 2 hours, and performing ultrasonic dispersion for 2 hours at the temperature of 70 ℃ to obtain a nano titanium dioxide dispersion system for later use.
(2) And (2) sequentially adding the alkaline compound dispersion system and the nano titanium dioxide dispersion system obtained in the step (1) into water, mixing and stirring for 90min at 60 ℃, finally adding the rest silane coupling agent KH550, stirring and reacting to be viscous at 70 ℃, drying for 20h at 110 ℃, and cooling to room temperature to obtain the desulfurizer.
(3) The desulfurizing agent was pulverized and ground into powder having a particle size of 600 nm by a pulverizer.
Example 2
A high-efficiency desulfurizer with an indicating function comprises the following components in parts by weight:
10 parts of zinc carbonate, 20 parts of basic copper carbonate, 10 parts of nano zinc oxide and 5 parts of a silane coupling agent KH 5505.
The preparation method of the desulfurizer comprises the following steps:
(1) adding zinc carbonate and basic copper carbonate into water with the initial temperature of 30 ℃, and uniformly stirring to obtain an alkaline compound dispersion system for later use; adding nano zinc oxide into water with the initial temperature of 50 ℃, adding 2 parts of silane coupling agent KH550, stirring for 2 hours, and performing ultrasonic dispersion at the temperature of 60 ℃ for 2 hours to obtain a nano zinc oxide dispersion system for later use.
(2) And (2) sequentially adding the alkaline compound dispersion system and the nano zinc oxide dispersion system obtained in the step (1) into water, mixing and stirring at 80 ℃ for 60min, finally adding the rest silane coupling agent KH550, stirring and reacting at 70 ℃ to be viscous, drying at 110 ℃ for 20h, and cooling to room temperature to obtain the desulfurizer.
(3) The desulfurizing agent was pulverized and ground into powder having a particle size of 1500 nm by a pulverizer.
Example 3
A high-efficiency desulfurizer with an indicating function comprises the following components in parts by weight:
10 parts of sodium carbonate, 40 parts of basic copper carbonate, 30 parts of nano magnesium oxide and 20 parts of amino silicone oil.
The preparation method of the desulfurizer comprises the following steps:
(1) adding sodium carbonate and basic copper carbonate into water with the initial temperature of 10 ℃, and uniformly stirring to obtain an alkaline compound dispersion system for later use; adding nano magnesium oxide into water with the initial temperature of 50 ℃, adding 10 parts of amino silicone oil, stirring for 2 hours, and performing ultrasonic dispersion for 1 hour at the temperature of 50 ℃ to obtain a nano magnesium oxide dispersion system for later use.
(2) And (2) sequentially adding the alkaline compound dispersion system and the nano magnesium oxide dispersion system obtained in the step (1) into water, mixing and stirring at 60 ℃ for 60min, finally adding the rest amino silicone oil, stirring and reacting at 50 ℃ to be viscous, drying at 80 ℃ for 15h, and cooling to room temperature to obtain the desulfurizer.
(3) The desulfurizing agent was pulverized and ground into powder having a particle size of 100 nm by a pulverizer.
Example 4
A high-efficiency desulfurizer with an indicating function comprises the following components in parts by weight:
30 parts of basic copper carbonate, 10 parts of nano-alumina and 20 parts of a silane coupling agent KH 55020.
The preparation method of the desulfurizer comprises the following steps:
(1) adding basic copper carbonate into water with the initial temperature of 30 ℃, and uniformly stirring to obtain an alkaline compound dispersion system for later use; adding nano-alumina into water with the initial temperature of 60 ℃, adding 10 parts of silane coupling agent KH550, stirring for 2 hours, and ultrasonically dispersing at the temperature of 60 ℃ for 1 hour to obtain a nano-alumina dispersion system for later use.
(2) And (2) sequentially adding the alkaline copper carbonate dispersion system and the nano aluminum oxide dispersion system obtained in the step (1) into water, mixing and stirring at 50 ℃ for 60min, finally adding the rest surface modifier, stirring and reacting at 70 ℃ to be viscous, drying at 100 ℃ for 6h, and cooling to room temperature to obtain the desulfurizer.
(3) The desulfurizing agent was pulverized and ground into powder having a particle size of 300 nm by a pulverizer.
Example 5
A high-efficiency desulfurizer with an indicating function comprises the following components in parts by weight:
60 parts of calcium hydroxide, 50 parts of basic copper carbonate, 10 parts of nano titanium dioxide and 25 parts of acetone.
The preparation method of the desulfurizer comprises the following steps:
(1) adding calcium hydroxide and basic copper carbonate into water with the initial temperature of 20 ℃, and uniformly stirring to obtain a calcium hydroxide dispersion system for later use; adding nano titanium dioxide into water with the initial temperature of 60 ℃, adding 10 parts of acetone, stirring for 1 hour, and performing ultrasonic dispersion for 1-2 hours at the temperature of 50 ℃ to obtain a nano titanium dioxide dispersion system for later use.
(2) And (2) sequentially adding the calcium hydroxide dispersion system and the nano titanium dioxide dispersion system obtained in the step (1) into water, mixing and stirring at 50 ℃ for 30min, finally adding the residual acetone, stirring and reacting at 50 ℃ to be viscous, drying at 100 ℃ for 5h, and cooling to room temperature to obtain the desulfurizer.
(3) The desulfurizing agent was pulverized and ground into powder having a particle size of 1000 nm by a pulverizer.
Example 6
A high-efficiency desulfurizer with an indicating function comprises the following components in parts by weight:
20 parts of basic zinc carbonate, 45 parts of basic copper carbonate, 10 parts of sodium hydroxide, 20 parts of nano zinc oxide, 25 parts of silane coupling agent KH550, 5 parts of activated carbon and 5 parts of diatomite.
The preparation method of the desulfurizer comprises the following steps:
(1) adding basic zinc carbonate, sodium hydroxide and basic copper carbonate into water with the initial temperature of 30 ℃, and uniformly stirring to obtain an alkaline compound dispersion system for later use; adding nano zinc oxide into water with the initial temperature of 60 ℃, adding 10 parts of silane coupling agent KH550, stirring for 1 hour, and ultrasonically dispersing at the temperature of 60 ℃ for 2 hours to obtain a nano zinc oxide dispersion system for later use.
(2) And (2) sequentially adding the alkaline compound dispersion system and the nano zinc oxide dispersion system obtained in the step (1) into water, mixing and stirring for 60min at 60 ℃, sequentially adding activated carbon and diatomite, continuously stirring for 90min, finally adding the rest silane coupling agent KH550, stirring and reacting to be viscous at 60 ℃, drying for 20h at 110 ℃, and cooling to room temperature to obtain the desulfurizer.
(3) The desulfurizing agent was pulverized and ground into powder having a particle size of 800 nm by a pulverizer.
Example 7
A high-efficiency desulfurizer with an indicating function comprises the following components in parts by weight:
20 parts of zinc carbonate, 30 parts of basic copper carbonate, 20 parts of nano titanium dioxide, 25 parts of amino silicone oil, 10 parts of activated carbon and 10 parts of diatomite.
The preparation method of the desulfurizer comprises the following steps:
(1) adding zinc carbonate and basic copper carbonate into water with the initial temperature of 30 ℃, and uniformly stirring to obtain an alkaline compound dispersion system for later use; adding nano titanium dioxide into water with the initial temperature of 60 ℃, adding 10 parts of amino silicone oil, stirring for 2 hours, and performing ultrasonic dispersion for 2 hours at the temperature of 70 ℃ to obtain a nano titanium dioxide dispersion system for later use.
(2) And (2) sequentially adding the alkaline compound dispersion system and the nano titanium dioxide dispersion system obtained in the step (1) into water, mixing and stirring for 60min at 90 ℃, sequentially adding active carbon and diatomite, continuously stirring for 90min, finally adding the rest amino silicone oil, stirring and reacting at 70 ℃ to be viscous, drying for 20h at 110 ℃, and cooling to room temperature to obtain the desulfurizer.
(3) The desulfurizing agent was pulverized and ground into powder having a particle size of 800 nm by a pulverizer.
Example 8
A high-efficiency desulfurizer with an indicating function comprises the following components in parts by weight:
60 parts of sodium silicate, 30 parts of basic copper carbonate, 30 parts of nano magnesium oxide, 25 parts of water-soluble silicone oil, 8 parts of active carbon and 6 parts of diatomite.
The sodium silicate in this example is solid sodium silicate with the molecular formula of Na2O·nSiO2The modulus n is 3.4, and the solubility solid is (omega/% > 99.0); besides, solid sodium silicate Na with modulus of 2.2-3.6 and soluble solid omega/% > 95.0 can also be adopted2O·nSiO2Effect and solid sodium silicate Na2O·nSiO2(n = 3.4) are the same.
The preparation method of the desulfurizer comprises the following steps:
(1) adding sodium silicate and basic copper carbonate into water with the initial temperature of 30 ℃, adding a dispersing agent and a hydrophobic agent, and uniformly stirring to obtain an alkaline compound dispersion system for later use; adding nano magnesium oxide into water with the initial temperature of 60 ℃, adding 10 parts of water-soluble silicone oil, stirring for 2 hours, and ultrasonically dispersing for 2 hours at the temperature of 60 ℃ to obtain a nano magnesium oxide dispersion system for later use.
(2) And (2) sequentially adding the alkaline compound dispersion system and the nano magnesium oxide dispersion system obtained in the step (1) into water, mixing and stirring for 60min at 90 ℃, sequentially adding active carbon and diatomite, continuously stirring for 90min, finally adding the rest water-soluble silicone oil, stirring and reacting to be viscous at 60 ℃, drying for 15h at 100 ℃, and cooling to room temperature to obtain the desulfurizer.
(3) The desulfurizing agent was pulverized and ground into powder having a particle size of 800 nm by a pulverizer.
Example 9
A high-efficiency desulfurizer with an indicating function comprises the following components in parts by weight:
10 parts of potassium hydroxide, 25 parts of basic copper carbonate, 10 parts of nano zinc oxide, 20 parts of acetone, 6 parts of activated carbon, 8 parts of diatomite and 2 parts of fumed silica.
The preparation method of the desulfurizer comprises the following steps:
(1) adding potassium hydroxide and basic copper carbonate into water with the initial temperature of 30 ℃, adding fumed silica, and uniformly stirring to obtain an alkaline compound dispersion system for later use; adding nano zinc oxide into water with the initial temperature of 60 ℃, adding 10 parts of acetone, stirring for 2 hours, and performing ultrasonic dispersion for 1 hour at the temperature of 50 ℃ to obtain a nano zinc oxide dispersion system for later use.
(2) And (2) sequentially adding the alkaline compound dispersion system and the nano zinc oxide dispersion system obtained in the step (1) into water, mixing and stirring for 30min at 25 ℃, sequentially adding active carbon and diatomite, continuously stirring for 60min, finally adding the rest acetone, stirring and reacting at 50 ℃ to be viscous, drying for 6h at 90 ℃, and cooling to room temperature to obtain the desulfurizer.
(3) The desulfurizing agent was pulverized and ground into powder having a particle size of 800 nm by a pulverizer.
Example 10
A high-efficiency desulfurizer with an indicating function comprises the following components in parts by weight:
45 parts of calcium hydroxide, 50 parts of basic copper carbonate, 25 parts of nano-alumina, 25 parts of ethanol, 5 parts of activated carbon and 5 parts of diatomite.
The preparation method of the desulfurizer comprises the following steps:
(1) adding calcium hydroxide and basic copper carbonate into water with the initial temperature of 30 ℃, and uniformly stirring to obtain an alkaline compound dispersion system for later use; adding nano alumina into water with the initial temperature of 50-60 ℃, adding 10 parts of ethanol, stirring for 1 hour, and performing ultrasonic dispersion for 1 hour at the temperature of 50 ℃ to obtain a nano alumina dispersion system for later use.
(2) And (2) sequentially adding the alkaline compound dispersion system and the nano-alumina dispersion system obtained in the step (1) into water, mixing and stirring for 30min at 10 ℃, sequentially adding active carbon and diatomite, continuously stirring for 60min, finally adding the rest ethanol, stirring and reacting at 50 ℃ to be viscous, drying for 8h at 80 ℃, and cooling to room temperature to obtain the desulfurizer.
(3) The desulfurizing agent was pulverized and ground into powder having a particle size of 800 nm by a pulverizer.
Example 11
A high-efficiency desulfurizer with an indicating function comprises the following components in parts by weight:
20 parts of basic zinc carbonate, 20 parts of basic copper carbonate, 20 parts of nano titanium dioxide, 20 parts of a silane coupling agent KH 55020 parts and 8 parts of methyl potassium silicate.
The preparation method of the desulfurizer comprises the following steps:
(1) adding basic zinc carbonate and basic copper carbonate into water with the initial temperature of 20 ℃, adding potassium methylsilicate, and uniformly stirring to obtain an alkaline compound dispersion system for later use; adding nano titanium dioxide into water with the initial temperature of 60 ℃, adding 10 parts of silane coupling agent KH550, stirring for 2 hours, and performing ultrasonic dispersion for 2 hours at the temperature of 70 ℃ to obtain a nano titanium dioxide dispersion system for later use.
(2) And (2) sequentially adding the alkaline compound dispersion system and the nano titanium dioxide dispersion system obtained in the step (1) into water, mixing and stirring for 90min at 60 ℃, finally adding the rest silane coupling agent KH550, stirring and reacting to be viscous at 70 ℃, drying for 20h at 110 ℃, and cooling to room temperature to obtain the desulfurizer.
(3) The desulfurizing agent was pulverized and ground into powder having a particle size of 600 nm by a pulverizer.
Example 12
A high-efficiency desulfurizer with an indicating function comprises the following components in parts by weight:
20 parts of basic zinc carbonate, 45 parts of basic copper carbonate, 10 parts of sodium hydroxide, 20 parts of nano zinc oxide, 25 parts of silane coupling agent KH550, 5 parts of activated carbon, 5 parts of diatomite and 2 parts of fumed silica.
The preparation method of the desulfurizer comprises the following steps:
(1) adding basic zinc carbonate, sodium hydroxide and basic copper carbonate into water with the initial temperature of 30 ℃, adding fumed silica, and uniformly stirring to obtain an alkaline compound dispersion system for later use; adding nano zinc oxide into water with the initial temperature of 60 ℃, adding 10 parts of silane coupling agent KH550, stirring for 1 hour, and ultrasonically dispersing at the temperature of 60 ℃ for 2 hours to obtain a nano zinc oxide dispersion system for later use.
(2) And (2) sequentially adding the alkaline compound dispersion system and the nano zinc oxide dispersion system obtained in the step (1) into water, mixing and stirring for 60min at 60 ℃, sequentially adding activated carbon and diatomite, continuously stirring for 90min, finally adding the rest silane coupling agent KH550, stirring and reacting to be viscous at 60 ℃, drying for 20h at 110 ℃, and cooling to room temperature to obtain the desulfurizer.
(3) The desulfurizing agent was pulverized and ground into powder having a particle size of 800 nm by a pulverizer.
Example 13
A high-efficiency desulfurizer with an indicating function comprises the following components in parts by weight:
20 parts of basic zinc carbonate, 6 parts of alkyl naphthalene sulfonate, 45 parts of basic copper carbonate, 10 parts of sodium hydroxide, 20 parts of nano zinc oxide, 25 parts of silane coupling agent KH550, 5 parts of activated carbon and 5 parts of diatomite.
The preparation method of the desulfurizer comprises the following steps:
(1) adding basic zinc carbonate, sodium hydroxide and basic copper carbonate into water with the initial temperature of 30 ℃, adding alkyl naphthalene sulfonate, and uniformly stirring to obtain an alkaline compound dispersion system for later use; adding nano zinc oxide into water with the initial temperature of 60 ℃, adding 10 parts of silane coupling agent KH550, stirring for 1 hour, and ultrasonically dispersing at the temperature of 60 ℃ for 2 hours to obtain a nano zinc oxide dispersion system for later use.
(2) And (2) sequentially adding the alkaline compound dispersion system and the nano zinc oxide dispersion system obtained in the step (1) into water, mixing and stirring for 60min at 60 ℃, sequentially adding activated carbon and diatomite, continuously stirring for 90min, finally adding the rest silane coupling agent KH550, stirring and reacting to be viscous at 60 ℃, drying for 20h at 110 ℃, and cooling to room temperature to obtain the desulfurizer.
(3) The desulfurizing agent was pulverized and ground into powder having a particle size of 800 nm by a pulverizer.
Example 14
A high-efficiency desulfurizer with an indicating function comprises the following components in parts by weight:
20 parts of basic zinc carbonate, 10 parts of polycarboxylate dispersant, 20 parts of basic copper carbonate, 20 parts of nano zinc oxide, 25 parts of silane coupling agent KH550, 5 parts of activated carbon, 5 parts of diatomite and 8 parts of fumed silica. The preparation method of the desulfurizer comprises the following steps:
(1) adding basic zinc carbonate and basic copper carbonate into water with the initial temperature of 30 ℃, adding a polycarboxylate dispersant and fumed silica, and uniformly stirring to obtain an alkaline compound dispersion system for later use; adding nano zinc oxide into water with the initial temperature of 60 ℃, adding 10 parts of silane coupling agent KH550, stirring for 2 hours, and performing ultrasonic dispersion for 2 hours at the temperature of 70 ℃ to obtain a nano zinc oxide dispersion system for later use.
(2) And (2) sequentially adding the alkaline compound dispersion system and the nano zinc oxide dispersion system obtained in the step (1) into water, mixing and stirring for 60min at 60 ℃, sequentially adding activated carbon and diatomite, continuously stirring for 60min, finally adding the rest silane coupling agent KH550, stirring and reacting to be viscous at 60 ℃, drying for 20h at 110 ℃, and cooling to room temperature to obtain the desulfurizer.
(3) The desulfurizing agent was pulverized and ground into powder having a particle size of 800 nm by a pulverizer.
Example 15
A high-efficiency desulfurizer with an indicating function comprises the following components in parts by weight:
20 parts of basic zinc carbonate, 2 parts of sodium polyacrylate, 20 parts of basic copper carbonate, 20 parts of nano zinc oxide, 5 parts of silane coupling agent KH 55025 parts of activated carbon, 5 parts of diatomite and 6 parts of methyl potassium silicate.
The preparation method of the desulfurizer comprises the following steps:
(1) adding basic zinc carbonate and basic copper carbonate into water with the initial temperature of 30 ℃, adding sodium polyacrylate and methyl potassium silicate, and uniformly stirring to obtain an alkaline compound dispersion system for later use; adding nano zinc oxide into water with the initial temperature of 60 ℃, adding 10 parts of silane coupling agent KH550, stirring for 2 hours, and performing ultrasonic dispersion for 2 hours at the temperature of 70 ℃ to obtain a nano zinc oxide dispersion system for later use.
(2) And (2) sequentially adding the alkaline compound dispersion system and the nano zinc oxide dispersion system obtained in the step (1) into water, mixing and stirring for 90min at the temperature of 60 ℃, sequentially adding active carbon and diatomite, continuously stirring for 60min, finally adding the rest silane coupling agent KH550, stirring and reacting at the temperature of 70 ℃ to be viscous, drying for 20h at the temperature of 100 ℃, and cooling to room temperature to obtain the desulfurizer.
(3) The desulfurizing agent was pulverized and ground into powder having a particle size of 800 nm by a pulverizer.
Comparative example 1
The desulfurizing agent in this comparative example was substantially the same in formulation and preparation method as those in example 1 except that basic copper carbonate was not added.
Comparative example 2
The desulfurizing agent in this comparative example was substantially the same in formulation and preparation method as those in example 6 except that diatomaceous earth was not added.
Comparative example 3
The desulfurizing agent in this comparative example was substantially the same in formulation and preparation method as those in example 6 except that activated carbon was not added.
Comparative example 4
The desulfurizing agent in this comparative example was substantially the same in formulation and preparation method as those in example 6 except that activated carbon and diatomaceous earth were not added.
Comparative example 5
The desulfurizing agent in this comparative example was substantially the same in formulation and preparation method as those in example 6 except that titanium dioxide having a particle size of 100 μm was used.
Performance test
1. The particle sizes of the desulfurizing agent products of examples 1 to 13 and comparative examples 1 to 5 were measured, and the results are shown in Table 1.
2. The desulfurizing agents of examples 1 to 13 and comparative examples 1 to 5 were prepared as saturated solutions, and the pH values of the saturated solutions were measured by a pH meter, and the results are shown in Table 1.
3. The water content measuring method comprises the following steps: a certain amount of a desulfurizing agent sample is weighed, and the ratio of the water lost after drying at 105-108 ℃ to the total mass of the sample is shown in Table 1.
4. According to the catching and eliminating efficiency experiment method in the reference standard Q/SHCG 122-2017 solid desulfurizer technical requirement, a penetrating sulfur capacity detection device is adopted, catching and eliminating agents with the weight of m are filled in a reaction tube desulfurizer section 4, and a total weighing pipe with the weight of m1Introducing hydrogen sulfide gas until the reaction is finished, and weighing the total pipe to be m2。
The catch-and-kill efficiency X was calculated as follows: x = [ (m)2−m1)/m]×100%。
The results of examining the hydrogen sulfide capturing efficiency of the desulfurizing agents of examples 1 to 13 and comparative examples 1 to 5 according to the above capturing efficiency test method are shown in Table 1.
TABLE 1
| Detecting items | Product particle size/mum | Saturated solution pH/(25 ℃ C.) | Water content% | Efficiency X/% of hydrogen sulfide elimination |
| Standard requirements | ≤1.5 | ≥11 | ≤3 | ≥95 |
| Example 1 | 1.3 | 11.86 | 2.1 | 98.2 |
| Example 2 | 1.0 | 11.23 | 2.1 | 98.0 |
| Example 3 | 1.2 | 11.56 | 2.3 | 98.6 |
| Example 4 | 1.4 | 11.38 | 2.5 | 97.7 |
| Example 5 | 1.3 | 11.22 | 2.0 | 97.5 |
| Example 6 | 0.8 | 12.32 | 1.9 | 99.5 |
| Example 7 | 0.9 | 11.88 | 1.9 | 99.2 |
| Example 8 | 0.9 | 11.76 | 2.2 | 97.5 |
| Example 9 | 1.1 | 12.19 | 2.2 | 99.1 |
| Example 10 | 1.2 | 11.52 | 2.7 | 96.3 |
| Example 11 | 1.0 | 11.74 | 1.9 | 97.6 |
| Example 12 | 0.9 | 12.07 | 1.7 | 99.1 |
| Example 13 | 0.8 | 12.88 | 2.3 | 98.7 |
| Example 14 | 0.8 | 12.10 | 1.7 | 99.2 |
| Example 15 | 0.8 | 12.29 | 1.8 | 98.6 |
| Comparative example 1 | 1.1 | 12.02 | 2.2 | 97.6 |
| Comparative example 2 | 1.3 | 11.92 | 2.0 | 96.8 |
| Comparative example 3 | 1.2 | 11.79 | 2.0 | 96.7 |
| Comparative example 4 | 1.2 | 11.68 | 1.9 | 95.9 |
| Comparative example 5 | 1.4 | 11.88 | 1.8 | 96.2 |
5. Analysis of results
(1) The product granularity, the pH value of a saturated solution, the water content and the catching and eliminating efficiency of hydrogen sulfide of the desulfurizing agent in the embodiments 1 to 15 all meet the standard requirements; as can be seen from the comparison of the capturing and eliminating efficiencies of the desulfurizing agents in example 6 and comparative examples 2 to 4, the absorption treatment efficiency of the desulfurizing agent on hydrogen sulfide is greatly improved by adding the diatomite and the activated carbon.
(2) When the desulfurizing agents of example 1 and comparative example 1 are used for hydrogen sulfide elimination, respectively, since a certain amount of basic copper carbonate is added to the desulfurizing agent formulation of example 1, a black substance (copper sulfide) is generated after the desulfurizing agent reacts with hydrogen sulfide, it can be judged whether hydrogen sulfide is completely eliminated (no black substance is generated, that is, hydrogen sulfide is completely eliminated), while it cannot be judged whether hydrogen sulfide is completely eliminated by using the desulfurizing agent of comparative example 1. Meanwhile, as can be seen from the comparison between the capturing and eliminating efficiencies of the example 1 and the comparative example 1 in the table 1, the absorption and treatment efficiency of the desulfurizing agent to the hydrogen sulfide can be improved by adding the basic copper carbonate.
(3) As can be seen from the comparison between example 6 and comparative example 5, the nano powder is adopted in the formula, and the specific surface area of the nano powder is increased after the nano powder is subjected to ultrasonic dispersion treatment, so that the reaction efficiency of the desulfurizing agent and the hydrogen sulfide can be effectively improved, and the absorption effect is improved.
(4) As is clear from the comparison between example 1 and example 11, and between example 6 and example 12, the water content of the desulfurizing agent in example 1 is higher than that in example 11, and the water content of the desulfurizing agent in example 6 is higher than that in example 12, and the above results indicate that the defect that the basic compound (such as basic zinc carbonate) is liable to absorb water can be effectively overcome by using the water repellent agent.
(5) As can be seen from the comparison between example 6 and example 13, the pH value of the saturated solution of the desulfurizing agent in example 6 is lower than that in example 13, and the above results show that the addition of the dispersing agent is beneficial to promoting the adjustment of the pH value of the alkaline compound and improving the suspension effect of the final product in the air.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (6)
1. The high-efficiency desulfurizer with the indicating function is characterized by comprising the following components in parts by weight: 10-60 parts of alkaline compound, 20-50 parts of basic copper carbonate, 10-30 parts of nano powder, 0-25 parts of surface modifier, 2-10 parts of dispersant and 2-8 parts of hydrophobic agent; or 10-60 parts of alkaline compound, 20-50 parts of basic copper carbonate, 10-30 parts of nano powder, 0-25 parts of surface modifier, 2-10 parts of dispersant, 2-8 parts of hydrophobic agent and 5-10 parts of active carbon; or 10-60 parts of alkaline compound, 20-50 parts of basic copper carbonate, 10-30 parts of nano powder, 0-25 parts of surface modifier, 2-10 parts of dispersant, 2-8 parts of hydrophobic agent and 5-10 parts of diatomite; or 10-60 parts of alkaline compound, 20-50 parts of basic copper carbonate, 10-30 parts of nano powder, 0-25 parts of surface modifier, 2-10 parts of dispersant, 2-8 parts of hydrophobic agent, 5-10 parts of activated carbon and 5-10 parts of diatomite;
in the desulfurizing agent, the weight part of the surface modifier does not contain 0 part;
the alkaline compound is selected from at least one of zinc carbonate, basic zinc carbonate, sodium silicate, potassium hydroxide, sodium hydroxide and calcium hydroxide;
the nano powder is selected from at least one of nano magnesium oxide, nano zinc oxide, nano aluminum oxide and nano titanium dioxide; the surface modifier is selected from at least one of amino silicone oil, a silane coupling agent HD110, a silane coupling agent KH550, a silane coupling agent KH570, water-soluble silicone oil, acetone and ethanol;
the dispersant is at least one selected from polycarboxylate dispersant, alkyl naphthalene sulfonate and sodium polyacrylate;
the hydrophobic agent is at least one of potassium methyl silicate and fumed silica;
the desulfurizer is powdery solid, and the pH of a saturated solution of the desulfurizer is more than or equal to 11;
the preparation method of the desulfurizing agent comprises the following steps:
(1) adding an alkaline compound and basic copper carbonate into water, adding a hydrophobic agent and a dispersing agent, and stirring and dispersing to obtain an alkaline compound dispersion system; dissolving the nano powder in water, adding part of surface modifier, stirring uniformly, and then performing ultrasonic dispersion to obtain a nano powder dispersion system;
(2) sequentially adding the alkaline compound dispersion system and the nano powder dispersion system obtained in the step (1) into water, uniformly stirring, finally adding the rest surface modifier, stirring and reacting to be viscous, and finally drying, cooling and grinding to obtain the desulfurizer;
when the desulfurizer also comprises activated carbon and/or diatomite, in the step (2), the alkaline compound dispersion system and the nano powder dispersion system are uniformly stirred, the activated carbon and/or diatomite are sequentially added, and the surface modifier is added after the uniform stirring.
2. The desulfurizing agent according to claim 1, wherein: the particle size of the nano powder is 100-300 nanometers.
3. The desulfurizing agent according to claim 1, wherein: the particle size of the desulfurizer is 100-1500 nm.
4. A method for preparing a high efficiency desulfurizing agent with indicating function according to any one of claims 1-3, characterized by comprising the steps of:
(1) adding an alkaline compound and basic copper carbonate into water, adding a hydrophobic agent and a dispersing agent, and stirring and dispersing to obtain an alkaline compound dispersion system; dissolving the nano powder in water, adding part of surface modifier, stirring uniformly, and then performing ultrasonic dispersion to obtain a nano powder dispersion system;
(2) sequentially adding the alkaline compound dispersion system and the nano powder dispersion system obtained in the step (1) into water, uniformly stirring, finally adding the rest surface modifier, stirring and reacting to be viscous, and finally drying, cooling and grinding to obtain the desulfurizer;
when the desulfurizer also comprises activated carbon and/or diatomite, in the step (2), the alkaline compound dispersion system and the nano powder dispersion system are uniformly stirred, the activated carbon and/or diatomite are sequentially added, and the surface modifier is added after the uniform stirring.
5. The method of claim 4, wherein: in the step (1), the initial temperature of water for dispersing the alkaline compound is 10-30 ℃, the initial temperature of water for dispersing the nano powder is 50-60 ℃, and the water temperature for ultrasonic dispersion is 50-70 ℃;
and/or in the step (1), the time of ultrasonic dispersion is 1-2 hours;
and/or in the step (2), the stirring temperature of the alkaline compound dispersion system and the nanometer powder dispersion system is 10-90 ℃, and the stirring time is 30-90 min;
and/or, in the step (2), the drying temperature is 80-110 ℃, and the drying time is 5-24 hours.
6. The method of claim 4, wherein: and (3) crushing the desulfurizer obtained in the step (2) into powder with the granularity of 100-1500 nanometers.
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| CN1712500A (en) * | 2004-06-21 | 2005-12-28 | 煤炭科学研究总院 | High-temperature gas composite oxide desulfurizer and production thereof |
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| CN101648108B (en) * | 2009-09-21 | 2013-01-23 | 中国石油化工股份有限公司 | Hydrogen sulfide gas leakage scavenger |
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