阅读说明：本技术 一种氧化铜基常温脱硫剂的制备方法 (Preparation method of copper oxide-based normal-temperature desulfurizing agent ) 是由 杜忠杰 于 2021-08-23 设计创作，主要内容包括：本发明实施例提供了一种氧化铜基常温脱硫剂的制备方法,包括以下步骤：配制一定浓度的凹凸棒土浆液；将一定量的铜盐加入到所述凹凸棒土浆液中,形成含一定铜浓度的第一复配浆液,并在一定温度下不断搅拌；将所述第一复配浆液置于微波超声仪中进行超声搅拌,然后加入一定含量的碱溶液,形成第二复配浆液,继续搅拌陈化一定时间；对所述第二复配浆液进行抽滤、水洗、干燥,并置于马弗炉内在一定温度下焙烧一定时间,得到氧化铜基脱硫材料；对所述氧化铜基脱硫材料进行成型,得到氧化铜基常温脱硫剂。本发明能够有效提高脱硫精度。(The embodiment of the invention provides a preparation method of a copper oxide-based normal-temperature desulfurizer, which comprises the following steps: preparing attapulgite slurry with a certain concentration; adding a certain amount of copper salt into the attapulgite slurry to form a first compound slurry containing a certain copper concentration, and continuously stirring at a certain temperature; placing the first compound slurry into a microwave ultrasonic instrument for ultrasonic stirring, then adding a certain content of alkali solution to form a second compound slurry, and continuing stirring and aging for a certain time; carrying out suction filtration, washing and drying on the second compound slurry, and placing the second compound slurry in a muffle furnace to be roasted for a certain time at a certain temperature to obtain a copper oxide-based desulfurization material; and forming the copper oxide-based desulfurization material to obtain the copper oxide-based normal-temperature desulfurizer. The invention can effectively improve the desulfurization precision.)

1. The preparation method of the copper oxide-based normal-temperature desulfurizing agent is characterized by comprising the following steps of:

s100: preparing attapulgite slurry with a certain concentration;

s200: adding a certain amount of copper salt into the attapulgite slurry to form a first compound slurry containing a certain copper concentration, and continuously stirring at a certain temperature;

s300: placing the first compound slurry into a microwave ultrasonic instrument for ultrasonic stirring, then adding a certain content of alkali solution to form a second compound slurry, and continuing stirring and aging for a certain time;

s400: carrying out suction filtration, washing and drying on the second compound slurry, and placing the second compound slurry in a muffle furnace to be roasted for a certain time at a certain temperature to obtain a copper oxide-based desulfurization material;

s500: and forming the copper oxide-based desulfurization material to obtain the copper oxide-based normal-temperature desulfurizer.

2. The preparation method of the copper oxide-based normal temperature desulfurizing agent according to claim 1, wherein the concentration of the attapulgite slurry is 1-50%.

3. The preparation method of the copper oxide-based normal temperature desulfurizing agent according to claim 1, wherein the concentration of copper in the first compound slurry is 0.01-1 mol/L.

4. The preparation method of the copper oxide-based normal temperature desulfurizing agent according to claim 3, wherein the copper salt in the first compound slurry is at least one of copper sulfate, copper nitrate and copper chloride.

5. The method for preparing the copper oxide-based normal temperature desulfurizing agent according to claim 1, wherein the alkali salt in the second compound slurry is at least one of sodium carbonate, sodium hydroxide, ammonium bicarbonate, ammonia water and ammonium carbonate.

6. The preparation method of the copper oxide-based normal temperature desulfurizing agent according to claim 1, wherein the ultrasonic aging time in the S300 is 2 to 24 hours.

7. The preparation method of the copper oxide-based normal temperature desulfurizing agent according to claim 1, wherein the drying temperature in the S400 is 80-150 ℃.

8. The method for preparing the copper oxide-based normal temperature desulfurizing agent according to claim 1, wherein the roasting temperature in the S400 is 150-450 ℃.

Technical Field

The invention belongs to the technical field of preparation of a desulfurizer, and particularly relates to a preparation method of a copper oxide-based normal-temperature desulfurizer.

Background

The progress of science and technology cannot keep away from the consumption of energy, and the development and utilization of the energy have a direct promoting effect on the development of the science and technology. The BP2035 world energy prospect report indicates that the energy consumption will continue to increase greatly, and under the great trend of world energy consumption, the energy consumption of China will reach 60%. Particularly, efficient clean utilization of coal, petroleum and natural gas is urgent, and the inevitable problem is the sulfur-containing compound mainly containing hydrogen sulfide.

The presence of hydrogen sulfide can cause catalyst poisoning and equipment corrosion, thereby endangering human health. Especially in the chemical reaction process, the influence of hydrogen sulfide in each gas component on the production is very serious. The agent suitable for normal temperature fine desulfurization mainly comprises copper oxide series, zinc oxide series and partial iron series desulfurizing agents, and the desulfurizing precision of the copper series desulfurizing agents is the best from the aspect of the desulfurizing effect.

In the existing Chinese patent, CN104694172A discloses a preparation method of a gas desulfurizer which takes zinc ferrite as an active component. The invention is prepared by an ultrasonic-assisted coprecipitation method, the average effective sulfur capacity of the desulfurizer is more than 10 percent through determination, the utilization rate of effective components in the raw materials is more than 80 percent, but the desulfurization precision is general.

Disclosure of Invention

The embodiment of the invention aims to provide a preparation method of a copper oxide-based normal-temperature desulfurizing agent, aiming at effectively improving the desulfurization precision.

The technical scheme adopted by the invention is as follows:

the embodiment of the invention provides a preparation method of a copper oxide-based normal-temperature desulfurizer, which comprises the following steps:

s100: preparing attapulgite slurry with a certain concentration;

s200: adding a certain amount of copper salt into the attapulgite slurry to form a first compound slurry containing a certain copper concentration, and continuously stirring at a certain temperature;

s300: placing the first compound slurry into a microwave ultrasonic instrument for ultrasonic stirring, then adding a certain content of alkali solution to form a second compound slurry, and continuing stirring and aging for a certain time;

s400: carrying out suction filtration, washing and drying on the second compound slurry, and placing the second compound slurry in a muffle furnace to be roasted for a certain time at a certain temperature to obtain a copper oxide-based desulfurization material;

s500: and forming the copper oxide-based desulfurization material to obtain the copper oxide-based normal-temperature desulfurizer.

Further, the concentration of the attapulgite slurry is 1-50%.

Further, the concentration of copper in the first compound slurry is 0.01-1 mol/L.

Further, the copper salt in the first compound slurry is at least one of copper sulfate, copper nitrate and copper chloride.

Further, the alkali salt in the second compound slurry is at least one of sodium carbonate, sodium hydroxide, ammonium bicarbonate, ammonia water and ammonium carbonate.

Further, the ultrasonic aging time in the S300 is 2 to 24 hours.

Further, the drying temperature in the S400 is 80-150 ℃.

Further, the calcination temperature in S400 is 150-450 ℃.

The invention has the beneficial effects that:

firstly, preparing attapulgite slurry with a certain concentration; then adding a certain amount of copper salt into the attapulgite slurry to form a first compound slurry containing a certain copper concentration, and continuously stirring at a certain temperature; then placing the first compound slurry into a microwave ultrasonic instrument for ultrasonic stirring, then adding a certain content of alkali solution to form a second compound slurry, and continuing stirring and aging for a certain time; carrying out suction filtration, washing and drying on the second compound slurry, and placing the second compound slurry in a muffle furnace to be roasted for a certain time at a certain temperature to obtain a copper oxide-based desulfurization material; and finally, molding the copper oxide-based desulfurization material to obtain the copper oxide-based normal-temperature desulfurizer, wherein the desulfurization precision can be effectively improved by the preparation method.

In order to make the aforementioned and other objects, features and advantages of the invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the embodiments of the present invention will be described in detail and completely with reference to the accompanying drawings. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention.

The terms "first", "second", and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.

Example 1

The preparation method of the copper oxide-based normal-temperature desulfurizer provided by the embodiment of the invention comprises the following steps:

step S100: preparing 25% attapulgite slurry;

step S200: adding copper nitrate into the attapulgite slurry to form a first compound slurry with copper ion concentration of 0.1mol/L, and continuously stirring at 40 ℃;

step S300: placing the first compound slurry into a microwave ultrasonic instrument for ultrasonic stirring for 2 hours, then adding a certain content of sodium hydroxide solution to form second compound slurry, enabling the pH value of the second compound slurry to be 7.5, and continuing stirring and aging for 5 hours;

step S400: carrying out suction filtration and water washing on the second compound slurry, and drying at 120 ℃ to constant weight; then placing the mixture in a muffle furnace to be roasted for 3 hours at the temperature of 300 ℃ to obtain a copper oxide-based desulfurization material;

step S500: and adding a binder into the copper oxide-based desulfurization material and forming the copper oxide-based normal-temperature desulfurizer.

Example 2

The preparation method of the copper oxide-based normal-temperature desulfurizer provided by the embodiment of the invention comprises the following steps:

step S100: preparing 30% attapulgite slurry;

step S200: adding copper chloride into the attapulgite slurry to form a first compound slurry with copper ion concentration of 0.2mol/l, and continuously stirring at 70 ℃;

step S300: placing the first compound slurry into a microwave ultrasonic instrument for ultrasonic stirring for 5 hours, then adding a sodium carbonate solution with a certain content to form second compound slurry, enabling the pH value of the second compound slurry to be 8, and continuing stirring and aging for 5 hours;

step S400: carrying out suction filtration, water washing and drying at 90 ℃ to constant weight on the second compound slurry; then placing the mixture in a muffle furnace and roasting the mixture for 2 hours at the temperature of 250 ℃ to obtain a copper oxide-based desulfurization material;

step S500: and adding a binder into the copper oxide-based desulfurization material to form the copper oxide-based normal-temperature desulfurizer.

Activity evaluation example

The evaluation steps of the desulfurizer prepared by the method of the invention are as follows:

drying the product at 90 ℃ for 2 hours, grinding and sieving the product by a sieve with 80-100 meshes, and accurately weighing 1g (with an accurate value of 0.0001 g) of sample;

filling the sample into a glass reaction tube, filling quartz sand with 60 meshes at two ends, and connecting hydrogen sulfide (with the concentration of 500 mg/m) at one end of the reaction tube³And the balance of nitrogen), one end of the reactor is connected with a gas chromatography test outlet to test the content of hydrogen sulfide. Opening the switch to introduce hydrogen sulfide gas, controlling the gas flow rate at 50ml/min, and detecting the content of hydrogen sulfide at the outlet of the chromatographic column to be more than 0.05mg/m³When the reaction is completed, the reaction is stopped.

The desulfurization activity of the product prepared in the above example was tested as shown in table 1:

TABLE 1 desulfurization Performance of copper oxide-based desulfurizing agent

Product(s)	Example 1	Example 2
			Sulfur capacity%	17	20

As can be seen from the above table, the desulfurizer of this type has excellent sulfur capacity at one time penetration and desulfurization precision.

In summary, the embodiment of the invention prepares the attapulgite slurry with a certain concentration; then adding a certain amount of copper salt into the attapulgite slurry to form a first compound slurry containing a certain copper concentration, and continuously stirring at a certain temperature; then placing the first compound slurry into a microwave ultrasonic instrument for ultrasonic stirring, then adding a certain content of alkali solution to form a second compound slurry, and continuing stirring and aging for a certain time; carrying out suction filtration, washing and drying on the second compound slurry, and placing the second compound slurry in a muffle furnace to be roasted for a certain time at a certain temperature to obtain a copper oxide-based desulfurization material; and finally, molding the copper oxide-based desulfurization material to obtain the copper oxide-based normal-temperature desulfurizer, wherein the desulfurization precision can be effectively improved by the preparation method.

The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.