CN111774044A - Regeneration method of protein soil adsorbent - Google Patents
Regeneration method of protein soil adsorbent Download PDFInfo
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- CN111774044A CN111774044A CN202010487407.7A CN202010487407A CN111774044A CN 111774044 A CN111774044 A CN 111774044A CN 202010487407 A CN202010487407 A CN 202010487407A CN 111774044 A CN111774044 A CN 111774044A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
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Abstract
A regeneration method of a protein soil adsorbent comprises the following steps: roasting the saturated adsorption opal for 30-100 min at 300-700 ℃ to obtain roasted opal, wherein the saturated adsorption opal is opal adsorbed with methylene blue; mixing Na2SO4Mixing with KOH solution to obtain mixed solution I, adding Ca (OH)2Mixing with glycerol solution to obtain mixed solution II; uniformly mixing the roasted opal with the mixed solution I to obtain a mixed material, and uniformly mixing the mixed material with the mixed solution II to obtain slurry; heating the slurry to 50-90 ℃, stirring and reacting for 3-10 h to obtain a reaction product, and drying and dehydrating the reaction product to obtain a finished product. The invention removes organic pollutants adsorbed by the opal through roasting saturated adsorption opal and hot solution treatment, retains the adsorption performance of the opal as much as possible, and realizes the recycling of the opal adsorbent.
Description
Technical Field
The invention belongs to the technical field of non-metallic mineral material deep processing and environmental engineering, and particularly relates to a regeneration method of a protein soil adsorbent.
Background
The protein soil is siliceous ore with rich reservesThe main production places of egg white clay in the world are Brazil, America, Mexico and the like, and the main production places in China are Henan, Shanxi, Yunnan, Jiangsu and the like. The opal is an aqueous amorphous or colloidal active silicon dioxide, the main chemical composition of which is SiO2、Al2O3、Fe2O3、TiO2The egg white soil also contains a small amount of MgO, CaO, organic matter, and the like, and varies depending on the place of production. The opal soil is hard in texture, large in specific surface area, high in porosity, rich in active hydroxyl on the surface and strong in adsorbability, and can adsorb toxic and harmful gases and elements, so that the opal soil is wide in application field and can be used for filter aids, decolorization adsorbents, stabilizers for paper pulp bleaching, inorganic fillers and the like.
However, in the adsorption process, the adsorption action of the opal is not performed any more after the opal reaches a saturated state, and the opal after the saturated adsorption becomes a harmful waste. However, replacement is not only likely to cause secondary pollution but also requires high replacement cost, and therefore, it is necessary to regenerate the opal after saturated adsorption. The regeneration technology can effectively realize the recycling of the protein soil, so that the protein soil can be recovered to the initial state before adsorption as far as possible, the life cycle of the protein soil adsorbent is prolonged, and the treatment cost is reduced.
At present, almost no regeneration treatment method for the protein soil after saturated adsorption exists, so that a regeneration method capable of recovering the adsorption performance of the protein soil is found, and the regeneration treatment method is very important for the regeneration and utilization of the protein soil adsorbent.
Disclosure of Invention
The invention aims to overcome the technical defects and provides a regeneration method of a protein soil adsorbent, which can remove organic pollutants adsorbed by the protein soil adsorbent and retain the adsorption performance of the protein soil adsorbent as far as possible.
In order to achieve the technical purpose, the technical scheme of the invention provides a method for regenerating a protein soil adsorbent, which comprises the following steps:
saturated adsorption opal soil is 300 to CRoasting at 700 ℃ for 30-100 min to obtain roasted opal, wherein the saturated adsorption opal is opal adsorbing methylene blue; mixing Na2SO4Mixing with KOH solution to obtain mixed solution I, adding Ca (OH)2Mixing with glycerol solution to obtain mixed solution II; uniformly mixing the roasted opal with the mixed solution I to obtain a mixed material, and uniformly mixing the mixed material with the mixed solution II to obtain slurry; heating the slurry to 50-90 ℃, stirring and reacting for 3-10 h to obtain a reaction product, and drying and dehydrating the reaction product to obtain a finished product.
Compared with the prior art, the invention has the beneficial effects that:
1. the regeneration method of the protein soil adsorbent provided by the invention comprises the steps of roasting saturated adsorption protein soil, then carrying out hot solution reaction treatment on the roasted protein soil in a mixed solution, wherein substances adsorbed in diatomite can be oxidized and volatilized, and part of adsorbed substances can be removed by the mixed solution; the main component of the opal is SiO2Roasting the opal soil and Na2SO4KOH solution, Na2SO4Provided with Na+Belonging to alkali metals with smaller atomic radius, Na+At OH-In the same way that the pores of the calcined opal are filled with KOH and Ca (OH)2Providing an alkaline environment required by the reaction cooperatively, easily opening the-Si-O-Si-bond on the surface of the roasted opal, and partially dissolving the surface of the roasted opal contacted with the mixed solution after reacting in an alkaline solution with a proper temperature for a certain time, so that the roughness of the surface of the roasted opal is increased, and the specific surface area of the roasted opal is increased; the alkaline solution environment and the glycerol can provide a large amount of-OH groups, so that part of-Si-O-Si-bonds on the surface of the roasted opal can be opened to form-Si-OH, namely, active hydroxyl groups are regenerated on the surface of the roasted opal, and the adsorption activity of the roasted opal is improved; in addition, a silicate phase generated by the reaction of the hot solution has abundant adsorption groups; the regeneration treatment method improves the roughness and the activity of the surface of the baked opal through the baking treatment and the hot solution treatment of the saturated adsorption opalThe organic pollutants adsorbed by the protein soil are removed, the adsorption performance of the protein soil is kept as much as possible, the recycling of the protein soil adsorbent is realized, and the cost of the adsorbent is reduced;
2. the regeneration method of the protein soil adsorbent provided by the invention is simple to operate, good in regeneration effect and low in raw material price, secondary pollution can be avoided in the regeneration process, and the protein soil adsorbent can be recycled and is environment-friendly.
Drawings
Fig. 1 is a process flow diagram of the method for regenerating the protein soil adsorbent of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Fig. 1 is a process flow diagram of a method for regenerating a protein soil adsorbent according to an embodiment of the present invention, and as shown in fig. 1, the embodiment of the present invention provides a method for regenerating a protein soil adsorbent, including the following steps:
roasting the saturated adsorption opal for 30-100 min at 300-700 ℃ to obtain roasted opal, wherein the saturated adsorption opal is opal adsorbed with methylene blue; mixing Na2SO4Mixing with KOH solution to obtain mixed solution I, adding Ca (OH)2Mixing with glycerol solution to obtain mixed solution II; uniformly mixing the roasted opal soil and the mixed solution I to obtain a mixed material, and uniformly mixing the mixed material and the mixed solution II to obtain slurry; heating the slurry to 50-90 ℃, stirring and reacting for 3-10 h to obtain a reaction product, and drying and dehydrating the reaction product to obtain a finished product.
In some preferred embodiments of the invention, Na is mixed in solution I2SO4The amount of the KOH is 2-12% of the mass of the roasted opal, and the amount of the KOH is 2-8% of the mass of the roasted opal; by optimizing Na2SO4And the amount of KOH,to ensure Na+And OH-Can fully act with the baking protein soil and avoid the waste of raw materials.
In some preferred embodiments of the invention, Ca (OH) in solution II is mixed2The content of the glycerol solution is 1-4% of the weight of the roasted opal, and the content of the glycerol solution is 2-4% of the weight of the roasted opal; by optimizing Ca (OH)2And glycerol in an amount to provide the OH necessary to provide a hot solution reaction-And avoids waste of raw materials.
In some preferred embodiments of the present invention, the calcined opal and the mixed solution I are mixed at a solid-to-liquid ratio of 1: 2-4, uniformly mixing; more preferably, the roasting opal and the mixed solution I are mixed according to a solid-to-liquid ratio of 1: 3, mixing uniformly.
In some preferred embodiments of the present invention, the mixture and the mixed solution II are mixed in a mass ratio of 1: 0.5-1.5 mixing uniformly; more preferably, the mass ratio of the mixed material to the mixed solution II is 1: 1, mixing uniformly.
In some preferred embodiments of the invention, after the mixed material is kept still for 10-30 min, the mixed material and the mixed solution II are uniformly mixed; to ensure that Na is filled in the pores on the surface of the roasted opal+And OH-Is favorable for opening the-Si-O-Si-bond on the surface of the roasted opal in the subsequent hot solution reaction process.
In some preferred embodiments of the invention, the slurry is heated after standing for 30-75 min; to ensure the sufficient contact between the baking opal and the mixed solution II to ensure that Ca (OH) is contained in the baking opal2And glycerol are fully acted on the roasted opal.
In some preferred embodiments of the invention, the stirring reaction rate is 100-250 r/min; the stirring reaction rate is optimized to increase the contact of the surface of the calcined opal and the mixed solution, and the mixed solution is diffused to the surface and the pore structure of the calcined opal as much as possible.
In some preferred embodiments of the present invention, the reaction product is washed to neutrality with pure water and then dried and dehydrated, and the dried and dehydrated reaction product is pulverized to a particle size of less than 74um, so as to obtain the finished product.
In the present invention, the temperature for drying and dehydrating the reaction product is not limited as long as it can ensure that the reaction product is dried and dehydrated, and for example, the reaction product can be dried and dehydrated at 100 ℃, and those skilled in the art can select an appropriate temperature for drying and dehydrating.
The mixed material is subjected to hot solution reaction in a closed environment, so that the volatilization of effective components in the mixed material is avoided.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The experimental methods in the present invention are conventional methods unless otherwise specified. The experimental materials used in the invention are all purchased in the market if no special description is provided; the opals in the following examples are from Qingdao (SiO)2Content 80%); na (Na)2SO4、KOH、Ca(OH)2And glycerol are analytically pure.
Example 1:
embodiment 1 of the present invention provides a method for regenerating a protein soil adsorbent, comprising the steps of:
(1) weighing opal (SiO) capable of adsorbing methylene blue in saturation2Content of 80%) in a crucible, placing the crucible in a muffle furnace for roasting at 600 ℃ for 40min, and cooling the roasted product to normal temperature after roasting to obtain roasted opal; weighing 9g of roasted opal, and stirring the roasted diatomite for 30min by using a vortex mixer to uniformly mix the diatomite for later use;
(2) respectively weighing Na accounting for 12 percent of the mass of the roasted opal2SO4KOH in an amount of 8% by mass of calcined opal, and Ca (OH) in an amount of 4% by mass of calcined opal2And glycerol with the mass of 4 percent of the baking opal, adding Na2SO4Mixing with KOH to obtain mixed solution I, adding Ca (OH)2Mixing with glycerol solution to obtain mixed solution II;
(3) and (3) mixing the roasted opal soil and the mixed solution I according to a solid-to-liquid ratio of 1: 3, uniformly mixing to obtain a mixed material, standing the mixed material for 20min, and mixing the mixed material with the mixed solution II according to a mass ratio of 1: 1, uniformly mixing to obtain slurry, standing the slurry for 50min, transferring the slurry into a water bath, heating the mixed material to 90 ℃, stirring and reacting for 10h at the stirring speed of 150r/min to obtain a reaction product, cooling the reaction product to normal temperature, washing the reaction product for 2-3 times by using pure water until the reaction product is neutral, drying and dehydrating the reaction product at 100 ℃, and crushing the dried and dehydrated reaction product to a particle size of less than 74um by using a powder grinding machine to obtain the regenerated protein soil adsorbent.
Example 2:
this example is essentially the same as example 1 with respect to the starting materials and preparation, except that: in the step (1), the roasting temperature is 300 ℃, and the roasting time is 100 min; when the mixed solution I and the mixed solution II are prepared in the step (2), Na accounting for 2 percent of the mass of the roasted opal is taken2SO4KOH in an amount of 2% by mass of calcined opal, and Ca (OH) in an amount of 1% by mass of calcined opal2And glycerol accounting for 2 percent of the mass of the roasted opal; the temperature of the hot solution in the step (3) is 70 ℃, and the reaction time is 3 h.
Example 3:
this example is essentially the same as example 1 with respect to the starting materials and preparation, except that: in the step (1), the roasting temperature is 400 ℃, and the roasting time is 80 min; when the mixed solution I and the mixed solution II are prepared in the step (2), Na accounting for 2 percent of the mass of the roasted opal is taken2SO4KOH in an amount of 8% by mass of calcined opal, and Ca (OH) in an amount of 4% by mass of calcined opal2And glycerol accounting for 4 percent of the mass of the roasted opal; the temperature of the hot solution in the step (3) is 90 ℃, and the reaction time is 10 h.
Example 4:
this example is essentially the same as example 1 with respect to the starting materials and preparation, except that: in the step (1), the roasting temperature is 500 ℃, and the roasting time is 60 min; when the mixed solution I and the mixed solution II are prepared in the step (2), taking Na with the mass of 12 percent of the roasting opal2SO4KOH with 2 percent of the mass of the baked opal, bakedCa (OH) accounting for 1% of the burned protein soil2And glycerol accounting for 4 percent of the mass of the roasted opal; the temperature of the hot solution in the step (3) is 85 ℃, and the reaction time is 7 h.
Example 5:
this example is essentially the same as example 1 with respect to the starting materials and preparation, except that: in the step (1), the roasting temperature is 700 ℃, and the roasting time is 30 min; when the mixed solution I and the mixed solution II are prepared in the step (2), taking Na with the mass of 12 percent of the roasting opal2SO4KOH in an amount of 8% by mass of calcined opal, and Ca (OH) in an amount of 1% by mass of calcined opal2And glycerol accounting for 2 percent of the mass of the roasted opal; the temperature of the hot solution in the step (3) is 90 ℃, and the reaction time is 8 h.
Example 6:
this example is essentially the same as example 1 with respect to the starting materials and preparation, except that: when the mixed solution I and the mixed solution II are prepared in the step (2), Na with the mass of 6 percent of the roasting opal is taken2SO4KOH in an amount of 5% by mass of calcined opal, and Ca (OH) in an amount of 2% by mass of calcined opal2And glycerol accounting for 4 percent of the mass of the roasted opal; the temperature of the hot solution in the step (3) is 85 ℃, and the reaction time is 7 h.
Comparative example 1:
the calcined opal prepared in example 1 was used as comparative example 1.
Comparative example 2:
this example is prepared essentially identically to example 1, except that: roasting the opal saturated for adsorbing methylene blue, and taking Na accounting for 2 percent of the mass of the opal when preparing the mixed solution I and the mixed solution II in the step (2)2SO4KOH in an amount of 8% by mass of the opal, and Ca (OH) in an amount of 4% by mass of the opal2And 4% glycerol by mass of the opal; the temperature of the hot solution in the step (3) is 90 ℃, and the reaction time is 10 h.
Comparative example 3:
this example is prepared essentially identically to example 1, except that: the opal saturated to adsorb the methylene blue is not roasted, and in the step (2)When preparing the mixed solution I and the mixed solution II, taking Na accounting for 2 percent of the mass of the opal2SO4KOH in an amount of 2% by mass of the opal, and Ca (OH) in an amount of 1% by mass of the opal2And glycerol accounting for 2 percent of the mass of the opal; the temperature of the hot solution in the step (3) is 70 ℃, and the reaction time is 3 h.
The adsorption amount of the regenerated protein soil adsorbents prepared in the embodiments 1 to 6 and the comparative examples 1 to 3 of the present invention to methylene blue and the specific surface area thereof were measured and used as evaluation indexes of products, and the test results are shown in table 1.
TABLE 1 Performance parameters of regenerated protein soil adsorbents prepared in examples 1 to 6 and comparative examples 1 to 3
As can be seen from Table 1, the regenerated protein soil adsorbents obtained in examples 1 to 6 and comparative examples 1 to 3 have a good adsorption amount of methylene blue, and the adsorption performance of the regenerated protein soil adsorbents can be recovered to 96.3% of that of the protein soil raw material at the highest, and the specific surface area can reach 62.25m at the highest2The fact that the recycling of the protein soil adsorbent can be effectively realized by the regeneration method is shown.
In order to verify that the regeneration method of the protein soil adsorbent provided by the invention is still effective after being circulated for multiple times, the inventor tests the methylene blue adsorption amount, the specific surface area and the ratio of the methylene blue adsorption amount to the raw ore adsorption amount of the protein soil adsorbent through multiple cycles, and specifically adopts the following method:
test subjects: selecting SiO2The content of the opal is 80 percent as the raw material;
the test method comprises the following steps: the same operation as in example 1 was carried out for a plurality of regeneration treatments.
The test results are shown in Table 2.
TABLE 2 Performance parameters of regenerated protein-soil adsorbents after regeneration multiple treatments
As can be seen from table 2, the regenerated opal still has good adsorption performance after being subjected to cyclic regeneration treatment, which indicates that the adoption of the regeneration treatment method of the invention can realize the repeated cyclic use of the opal adsorbent and effectively reduce the cost of the opal adsorbent.
The above-described embodiments of the present invention should not be construed as limiting the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the protection scope of the claims of the present invention.
Claims (9)
1. The regeneration method of the protein soil adsorbent is characterized by comprising the following steps: roasting the saturated adsorption opal for 30-100 min at 300-700 ℃ to obtain roasted opal, wherein the saturated adsorption opal is opal adsorbed with methylene blue; mixing Na2SO4Mixing with KOH solution to obtain mixed solution I, adding Ca (OH)2Mixing with glycerol solution to obtain mixed solution II; uniformly mixing the roasted opal with the mixed solution I to obtain a mixed material, and uniformly mixing the mixed material with the mixed solution II to obtain slurry; heating the slurry to 50-90 ℃, stirring and reacting for 3-10 h to obtain a reaction product, and drying and dehydrating the reaction product to obtain a finished product.
2. The method for regenerating a protein soil adsorbent as claimed in claim 1, wherein Na is contained in the mixed solution I2SO4The amount of the KOH is 2-12% of the mass of the roasted opal, and the amount of the KOH is 2-8% of the mass of the roasted opal.
3. The method for regenerating a protein-soil adsorbent as claimed in claim 1, wherein Ca (OH) in the mixed solution II2The amount of the glycerol solution is 1-4% of the mass of the calcined opal, and the amount of the glycerol solution is 2-4% of the mass of the calcined opal.
4. The regeneration method of a protein soil adsorbent according to claim 1, wherein the ratio of the calcined protein soil to the mixed solution I is 1: 2-4, and mixing uniformly.
5. The method for regenerating a protein soil adsorbent according to claim 1, wherein the mass ratio of the mixed material to the mixed solution II is 1: 0.5-1.5, and mixing uniformly.
6. The method for regenerating a protein soil adsorbent according to claim 1, wherein the mixed material is left to stand for 10-30 min and then mixed with the mixed solution II uniformly.
7. The method for regenerating a protein soil adsorbent according to claim 1, wherein the slurry is heated after being left to stand for 30 to 75 min.
8. The method for regenerating a protein soil adsorbent according to claim 1, wherein the stirring reaction rate is 100 to 250 r/min.
9. The method for regenerating a protein soil adsorbent according to claim 1, wherein the reaction product is washed to neutrality with pure water, and then dried and dehydrated, and the dried and dehydrated reaction product is pulverized to a particle size of less than 74um, and then the finished product is obtained.
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