CN107029684B - Slow-release type long-acting gas deoxidizer and preparation method thereof - Google Patents
Slow-release type long-acting gas deoxidizer and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a slow-release long-acting gas deoxidizer and a preparation method thereof, wherein the deoxidizer comprises 70% of a carrier and 30% of active components by weight, wherein the carrier comprises the following raw materials in parts by weight: 43-55 parts of zirconium oxide, 22-25 parts of talc, 18-21 parts of attapulgite, 15-19 parts of diatomite, 6-10 parts of hydroxypropyl cellulose, 16-20 parts of natural resin, 26-31 parts of crospovidone, 11-17 parts of calcium borate, 5-8 parts of quartz sand and 7-11 parts of water glass, wherein the active components comprise the following raw materials in molar ratio: MnO2：ZnO：TiO2：Y2O3：Nd2O31: 0.65-0.75: 0.2-0.4: 0.12-0.2: 0.25 to 0.3. The invention has the characteristics of high mechanical strength, deep deoxidation depth, difficult pulverization, high deoxidation capacity and long service life.
Description
Technical Field
The invention relates to the technical field of chemical deoxidation. More particularly, the invention relates to a slow-release type long-acting gas deoxidizer and a preparation method thereof.
Background
The deoxidation methods currently used in the chemical industry are mainly of two types: the first is catalytic hydrodeoxygenation, which uses some noble metals as catalysts, and introduces hydrogen to react with trace oxygen in target gas to generate water, the method has the greatest advantage of high activity at normal temperature, but the defects are also obvious, the first is high cost, the second is strict requirement on impurity gas in target gas, and ensures gas which cannot contain sulfur, chlorine and other components to prevent catalyst poisoning, so the method has little audience, the second is a more-used chemical absorption method, uses some metals with strong oxidizability as active components to react with trace oxygen in target gas to achieve the aim of deoxidation, and uses reducing gas to reduce the active components for reuse, the method has the advantages of low cost, but the deoxidizer in the method has some problems, and the first is poor mechanical strength and easy pulverization, secondly, the deoxidation depth is not enough, the three needles can not play a good deoxidation effect on gases possibly mixed with ammonia nitrogen or other active ingredients easy to poison, and the manganese series deoxidizer also has a unique defect that the temperature runaway in the reduction process is easy to further reduce the mechanical strength of the deoxidizer.
Disclosure of Invention
The invention aims to provide a slow-release long-acting gas deoxidizer which has high mechanical strength, deep deoxidation depth, difficult pulverization, high deoxidation capacity and long service life.
To achieve these objects and other advantages in accordance with the present invention, there is provided a slow-release type long-acting gas deoxidizer including 70% by weight of a carrier and 30% by weight of an active ingredient, wherein the carrier includes the following raw materials in parts by weight: 43-55 parts of zirconium oxide, 22-25 parts of talc, 18-21 parts of attapulgite, 15-19 parts of diatomite, 6-10 parts of hydroxypropyl cellulose, 16-20 parts of natural resin, 26-31 parts of crospovidone, 11-17 parts of calcium borate, 5-8 parts of quartz sand and 7-11 parts of water glass, wherein the active components comprise the following raw materials in molar ratio: MnO2：ZnO：TiO2：Y2O3：Nd2O3＝1：0.65～0.75：0.2～0.4：0.12～0.2：0.25～0.3。
Preferably, one or more of nickel oxide, cobalt oxide and chromium oxide is/are further added into the active component.
Preferably, the chromium oxide is CrO3With MnO of2In a molar ratio of 0.33 to 0.4: 1.
the invention also provides a preparation method of the slow-release type long-acting gas deoxidizer, which comprises the following steps:
crushing the zirconium oxide, the talc, the attapulgite, the diatomite, the hydroxypropyl cellulose, the calcium borate, the quartz sand and the crospovidone in parts by weight, and then sieving and uniformly mixing the crushed materials by using a 300-400-mesh sieve;
step two, adding the natural resin and the water glass in parts by weight into the mixture prepared in the step one, heating to 45-50 ℃, uniformly stirring, pressing into a cylindrical solid through a cylindrical die, and drying at the temperature of 80-90 ℃;
dissolving the active component in a dilute hydrochloric acid solution with the concentration of 5%, adjusting the pH value to 3-4, and then soaking the cylindrical solid prepared in the step two in the dilute hydrochloric acid solution containing the active component for 18-22 hours;
step four, naturally drying the cylindrical solid soaked in the step three, then hermetically wrapping the cylindrical solid by using a glass shell, roasting the cylindrical solid at 350-450 ℃ for 2-3 hours, uniformly rotating the cylindrical solid in the roasting process to uniformly heat the cylindrical solid, and breaking the glass shell after roasting is finished;
and step five, placing the cylindrical solid roasted in the step four in an atmosphere of hydrogen or carbon monoxide for reduction, wherein the gas flow rate is 250ml/s, the gas temperature is gradually increased from room temperature to 100-120 ℃, and the reduction time is 5.5-6 hours.
Preferably, the pressure for pressing by using the cylindrical die in the second step is 1.2-1.5 MPa.
Preferably, the soaking process of the cylindrical solid in the third step can be completed by adopting a siphon traction process, and the specific method comprises the following steps: the method comprises the steps of subpackaging dilute hydrochloric acid solution containing active components into two water tanks, wherein the height of one water tank is higher than that of the other water tank, the two water tanks are communicated in an inverted mode through a U-shaped pipe, a cylindrical solid is placed in a vertical pipe of the U-shaped pipe, and then the U-shaped pipe is filled with the dilute hydrochloric acid solution containing the active components to form a siphoning effect.
Preferably, the diameter of the vertical pipe of the U-shaped pipe is the same as the diameter of the cross section of the cylindrical solid.
The invention at least comprises the following beneficial effects:
1. the natural resin, the water glass and other components are added to fix the shapes of the zirconia, the talc, the attapulgite, the diatomite and other clays, so that the deoxidant is not damaged in the preparation process, the mechanical strength of the zirconia after roasting is high, and the porosity of the carrier is not greatly changed due to pressing or roasting processing.
2. The crospovidone, the hydroxypropyl cellulose and the active ingredients can be well matched to play a long-term and continuous deoxidation effect, and meanwhile, the defects that the manganese oxide is quickly oxidized by oxygen in the air after being reduced and the deoxidation capacity is reduced are avoided.
3. The yttrium and neodymium elements are added to protect the manganese from being poisoned by ammonia nitrogen or other gases, so that the deoxidation effect is reduced, and the service life of the deoxidizer is prolonged.
4. When the deoxidizer is subjected to reduction pretreatment, the generated sudden temperature rise can transfer heat to some low-melting-point substances so as to protect a porous framework formed by the clay from being pulverized by high temperature, and meanwhile, the high porosity of the deoxidizer can quickly conduct high temperature to the air.
5. The micro-corrosion treatment of the hydrochloric acid aerial fog can increase the porosity of the cylindrical solid formed by the carrier, adsorb more transitional components and further improve the deoxidation effect.
6. The addition of chromium to the active ingredient further increases the deoxidizing effect of the deoxidizer and the temperature breadth of use.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
It is to be noted that the experimental methods described in the following embodiments are all conventional methods unless otherwise specified, and the reagents and materials are commercially available unless otherwise specified.
< example 1 >:
a slow-release long-acting gas deoxidizer comprises 70% of a carrier and 30% of an active component by weight percent, wherein the carrier comprises the following raw materials in parts by weight: 43 parts of zirconium oxide, 22 parts of talc, 18 parts of attapulgite, 15 parts of diatomite, 6 parts of hydroxypropyl cellulose, 16 parts of natural resin, 26 parts of crospovidone, 11 parts of calcium borate, 5 parts of quartz sand and 7 parts of water glass, wherein the active components comprise the following raw materials in molar ratio: MnO2：ZnO：TiO2：Y2O3：Nd2O3：CrO3＝1：0.65：0.2：0.12：0.25：0.33。
The preparation method of the slow-release long-acting gas deoxidizer comprises the following steps:
crushing the zirconium oxide, the talc, the attapulgite, the diatomite, the hydroxypropyl cellulose, the calcium borate, the quartz sand and the crospovidone in parts by weight, and then sieving and uniformly mixing the crushed materials by using a 300-mesh sieve;
step two, adding the natural resin and the water glass in parts by weight into the mixture prepared in the step one, heating to 45 ℃, uniformly stirring, pressing into a cylindrical solid through a cylindrical die, wherein the pressing pressure is 1.2MPa, drying at the temperature of 80 ℃, and then placing the cylindrical solid into hydrochloric acid aerial fog for surface micro-corrosion treatment;
step three, dissolving the active component in a dilute hydrochloric acid solution with the concentration of 5%, adjusting the pH value to 3, then soaking the cylindrical solid prepared in the step two in the dilute hydrochloric acid solution containing the active component for 18 hours, wherein the soaking process is completed by adopting a siphon traction process, and the specific method comprises the following steps: the method comprises the following steps of subpackaging dilute hydrochloric acid solution containing active components into two water tanks, wherein the height of one water tank is higher than that of the other water tank, the two water tanks are communicated in an inverted mode through a U-shaped pipe, a cylindrical solid is placed in a vertical pipe of the U-shaped pipe, then the U-shaped pipe is filled with the dilute hydrochloric acid solution containing the active components to form a siphoning effect, and the dilute hydrochloric acid solution containing the active components slowly permeates into pores of the cylindrical solid, wherein the inner diameter of the vertical pipe of the U-shaped pipe is the same as the diameter of the section of the cylindrical solid;
step four, naturally drying the cylindrical solid soaked in the step three, then sealing and wrapping the cylindrical solid by using a glass shell, roasting the cylindrical solid at 350 ℃ for 2 hours, uniformly rotating the cylindrical solid in the roasting process to ensure uniform heating, and breaking the glass shell after roasting is finished;
and step five, placing the cylindrical solid roasted in the step four in an atmosphere of hydrogen or carbon monoxide for reduction, wherein the gas flow rate is 250ml/s, the gas temperature is gradually increased from room temperature to 100 ℃, and the reduction time is 5.5 hours.
< example 2 >:
a kind of slowThe release type long-acting gas deoxidizer comprises 70 percent of carrier and 30 percent of active component by weight percent, wherein the carrier comprises the following raw materials in parts by weight: 55 parts of zirconium oxide, 25 parts of talcum, 21 parts of attapulgite, 19 parts of diatomite, 10 parts of hydroxypropyl cellulose, 20 parts of natural resin, 31 parts of crospovidone, 17 parts of calcium borate, 8 parts of quartz sand and 11 parts of water glass, wherein the active components comprise the following raw materials in molar ratio: MnO2：ZnO：TiO2：Y2O3：Nd2O3：CrO3＝1：0.75：0.4：0.2：0.3：0.4。
The preparation method of the slow-release long-acting gas deoxidizer comprises the following steps:
crushing the zirconium oxide, the talc, the attapulgite, the diatomite, the hydroxypropyl cellulose, the calcium borate, the quartz sand and the crospovidone in parts by weight, and then sieving and uniformly mixing the crushed materials by using a 400-mesh sieve;
step two, adding the natural resin and the water glass in parts by weight into the mixture prepared in the step one, heating to 50 ℃, uniformly stirring, pressing into a cylindrical solid through a cylindrical die, wherein the pressing pressure is 1.5MPa, drying at the temperature of 90 ℃, and then placing the cylindrical solid into hydrochloric acid aerial fog for surface micro-corrosion treatment;
step three, dissolving the active component in a dilute hydrochloric acid solution with the concentration of 5%, adjusting the pH value to 4, then soaking the cylindrical solid prepared in the step two in the dilute hydrochloric acid solution containing the active component for 22 hours, wherein the soaking process is completed by adopting a siphon traction process, and the specific method comprises the following steps: the method comprises the following steps of subpackaging dilute hydrochloric acid solution containing active components into two water tanks, wherein the height of one water tank is higher than that of the other water tank, the two water tanks are communicated in an inverted mode through a U-shaped pipe, a cylindrical solid is placed in a vertical pipe of the U-shaped pipe, then the U-shaped pipe is filled with the dilute hydrochloric acid solution containing the active components to form a siphoning effect, and the dilute hydrochloric acid solution containing the active components slowly permeates into pores of the cylindrical solid, wherein the inner diameter of the vertical pipe of the U-shaped pipe is the same as the diameter of the section of the cylindrical solid;
step four, naturally drying the cylindrical solid soaked in the step three, then sealing and wrapping the cylindrical solid by using a glass shell, roasting the cylindrical solid at 450 ℃ for 3 hours, uniformly rotating the cylindrical solid in the roasting process to ensure uniform heating, and breaking the glass shell after roasting is finished;
and step five, placing the cylindrical solid roasted in the step four in an atmosphere of hydrogen or carbon monoxide for reduction, wherein the gas flow rate is 250ml/s, the gas temperature is gradually increased from room temperature to 120 ℃, and the reduction time is 6 hours.
< example 3 >:
a slow-release long-acting gas deoxidizer comprises 70% of a carrier and 30% of an active component by weight percent, wherein the carrier comprises the following raw materials in parts by weight: 49 parts of zirconium oxide, 23.5 parts of talc, 19.5 parts of attapulgite, 17 parts of diatomite, 8 parts of hydroxypropyl cellulose, 18 parts of natural resin, 28.5 parts of crospovidone, 14 parts of calcium borate, 6.5 parts of quartz sand and 9 parts of water glass, wherein the active components comprise the following raw materials in mol ratio: MnO2：ZnO：TiO2：Y2O3：Nd2O3：CrO3＝1：0.7：0.3：0.16：0.27：0.36。
The preparation method of the slow-release long-acting gas deoxidizer comprises the following steps:
crushing the zirconium oxide, the talc, the attapulgite, the diatomite, the hydroxypropyl cellulose, the calcium borate, the quartz sand and the crospovidone in parts by weight, and then sieving and uniformly mixing the crushed materials by using a 350-mesh sieve;
step two, adding the natural resin and the water glass in parts by weight into the mixture prepared in the step one, heating to 48 ℃, uniformly stirring, pressing into a cylindrical solid through a cylindrical die, wherein the pressing pressure is 1.35MPa, drying at the temperature of 85 ℃, and then placing the cylindrical solid into hydrochloric acid aerial fog for surface micro-corrosion treatment;
step three, dissolving the active component in a dilute hydrochloric acid solution with the concentration of 5%, adjusting the pH value to 3.5, then soaking the cylindrical solid prepared in the step two in the dilute hydrochloric acid solution containing the active component for 20 hours, wherein the soaking process is finished by adopting a siphon traction process, and the specific method comprises the following steps: the method comprises the following steps of subpackaging dilute hydrochloric acid solution containing active components into two water tanks, wherein the height of one water tank is higher than that of the other water tank, the two water tanks are communicated in an inverted mode through a U-shaped pipe, a cylindrical solid is placed in a vertical pipe of the U-shaped pipe, then the U-shaped pipe is filled with the dilute hydrochloric acid solution containing the active components to form a siphoning effect, and the dilute hydrochloric acid solution containing the active components slowly permeates into pores of the cylindrical solid, wherein the inner diameter of the vertical pipe of the U-shaped pipe is the same as the diameter of the section of the cylindrical solid;
step four, naturally drying the cylindrical solid soaked in the step three, then sealing and wrapping the cylindrical solid by using a glass shell, roasting the cylindrical solid at the temperature of 410 ℃ for 2.5 hours, uniformly rotating the cylindrical solid in the roasting process to uniformly heat the cylindrical solid, and breaking the glass shell after the roasting is finished;
and step five, placing the cylindrical solid roasted in the step four in an atmosphere of hydrogen or carbon monoxide for reduction, wherein the gas flow rate is 250ml/s, and simultaneously gradually increasing the gas temperature from room temperature to 110 ℃ for 5.8 hours.
< comparative example 1 >:
a manganese-based deoxidizer was produced in the same manner as in example 3 except that zirconia, a natural resin and water glass were not contained in the deoxidizer, and the deoxidizer was produced in the same manner as in example 3.
< comparative example 2 >:
a manganese-based deoxidizer having the same composition as in example 3 except that Y is not contained2O3、Nd2O3、CrO3The preparation method is also the same as that of example 3.
The deoxidation effects of examples 1-3 and comparative examples 1-2 were tested separately, with the test gas consisting of 70% by volume of H220% of N25.8% of CO and 4% of SO2And 0.2% of O2The composition is tested at 5atm, room temperature, 5000hr-1The mechanical strength of examples 1 to 3 and comparative example were measured at the same time, and the results are shown in Table 1.
TABLE 1 comparative table of deoxidizing ability and mechanical strength of deoxidizing agent
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | |
| Mechanical strength | 14kg/cm2 | 13kg/cm2 | 16kg/cm2 | 4.2kg/cm2 | 13kg/cm2 |
| Depth of deoxidation | 0.07ppm | 0.08ppm | 0.01ppm | 0.1ppm | 1ppm |
| Capacity of deoxidation | 55ml/g | 59ml/g | 62ml/g | 56ml/g | 30ml/g |
As can be seen from Table 1, the deoxidizers of examples 1 to 3 were significantly superior in mechanical strength to those of comparative example 1, and in the deoxidation depth and the deoxidation capacity to those of comparative example 2.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable to various fields of endeavor for which the invention may be embodied with additional modifications as would be readily apparent to those skilled in the art, and the invention is therefore not limited to the details given herein and to the embodiments shown and described without departing from the generic concept as defined by the claims and their equivalents.
Claims (4)
1. The preparation method of the slow-release type long-acting gas deoxidizer is characterized in that the slow-release type long-acting gas deoxidizer comprises 70% of a carrier and 30% of an active component by weight percent, wherein the carrier comprises the following raw materials in parts by weight: 43-55 parts of zirconium oxide, 22-25 parts of talc, 18-21 parts of attapulgite, 15-19 parts of diatomite, 6-10 parts of hydroxypropyl cellulose, 16-20 parts of natural resin, 26-31 parts of crospovidone, 11-17 parts of calcium borate, 5-8 parts of quartz sand and 7-11 parts of water glass, wherein the active components comprise the following raw materials in molar ratio: MnO2：ZnO：TiO2：Y2O3：Nd2O31: 0.65-0.75: 0.2-0.4: 0.12-0.2: 0.25 to 0.3, CrO is also added into the active component3With MnO of2In a molar ratio of 0.33 to 0.4: 1;
the preparation method of the slow-release type long-acting gas deoxidizer comprises the following steps:
crushing the zirconium oxide, the talc, the attapulgite, the diatomite, the hydroxypropyl cellulose, the calcium borate, the quartz sand and the crospovidone in parts by weight, and then sieving and uniformly mixing the crushed materials by using a 300-400-mesh sieve;
step two, adding the natural resin and the water glass in parts by weight into the mixture prepared in the step one, heating to 45-50 ℃, uniformly stirring, pressing into a cylindrical solid through a cylindrical die, drying at 80-90 ℃, and placing the cylindrical solid into hydrochloric acid aerial fog for surface micro-corrosion treatment;
dissolving the active component in a dilute hydrochloric acid solution with the concentration of 5%, adjusting the pH value to 3-4, and then soaking the cylindrical solid prepared in the step two in the dilute hydrochloric acid solution containing the active component for 18-22 hours;
step four, naturally drying the cylindrical solid soaked in the step three, then hermetically wrapping the cylindrical solid by using a glass shell, roasting the cylindrical solid at 350-450 ℃ for 2-3 hours, uniformly rotating the cylindrical solid in the roasting process to uniformly heat the cylindrical solid, and breaking the glass shell after roasting is finished;
and step five, placing the cylindrical solid roasted in the step four in an atmosphere of hydrogen or carbon monoxide for reduction, wherein the gas flow rate is 250ml/s, the gas temperature is gradually increased from room temperature to 100-120 ℃, and the reduction time is 5.5-6 hours.
2. The method for preparing a sustained-release long-acting gas deoxidizer according to claim 1, wherein the pressure for pressing by using a cylindrical mold in the second step is 1.2 to 1.5 MPa.
3. The preparation method of the slow-release long-acting gas deoxidizer of claim 1 is characterized in that the soaking process of the cylindrical solid in the step three is completed by adopting a siphon traction process, and the specific method comprises the following steps: the method comprises the steps of subpackaging dilute hydrochloric acid solution containing active components into two water tanks, wherein the height of one water tank is higher than that of the other water tank, the two water tanks are communicated in an inverted mode through a U-shaped pipe, a cylindrical solid is placed in a vertical pipe of the U-shaped pipe, and then the U-shaped pipe is filled with the dilute hydrochloric acid solution containing the active components to form a siphoning effect.
4. The method for producing a sustained-release long-acting gas deoxidizer of claim 3, wherein the vertical tube diameter of the U-shaped tube is the same as the cross-sectional diameter of the cylindrical solid.
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