CN113321231B - Method for preparing calcite by herbaceous plant induction - Google Patents
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- CN113321231B CN113321231B CN202110607996.2A CN202110607996A CN113321231B CN 113321231 B CN113321231 B CN 113321231B CN 202110607996 A CN202110607996 A CN 202110607996A CN 113321231 B CN113321231 B CN 113321231B
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Abstract
The invention relates to a method for preparing calcite by inducing herbaceous plants, and belongs to the technical field of calcite synthesis. The method for preparing calcite by inducing herbaceous plants comprises the following steps: dispersing powder of herbaceous plants in water, reacting for 6-12 h at 200-220 ℃, and carrying out solid-liquid separation to obtain a carbon quantum dot solution, wherein the concentration of the carbon quantum dot solution is 20-25 g/L; mixing the carbon quantum dot solution and a soluble calcium salt solution to obtain a mixed solution, adding a soluble carbonate solution at a rate of 4-5 mL/min to react for 1.9-2.2 h, filtering, washing and drying to obtain calcite; wherein the herbaceous plant is at least one of alligator alternanthera or alligator alternanthera; the pH value of the carbon quantum dot solution is 6.9-10.35. According to the invention, the utilization value of the calcite is improved by using the invasive plants to prepare the calcite. The SEM picture of the calcite prepared by the method shows that the calcite has a flower-shaped structure with square petals and is high in purity.
Description
Technical Field
The invention relates to a method for preparing calcite by inducing herbaceous plants, and belongs to the technical field of calcite synthesis.
Background
Calcite is a calcium carbonate mineral, the crystal shape of calcite is various, and a plurality of square fragments can be obtained by knocking the calcite, so the calcite is famous and famous. The color of calcite varies depending on the impurities contained therein, e.g. pale yellow, pale red, brownish black, etc. in the case of iron and manganese, but is generally white or colorless. Colorless transparent calcite, also known as icentine, has a wonderful feature that objects can be seen through it in a double image. Thus, ice is an important optical material. Calcite has many uses in production and life. Limestone is known to form karst caves, and stalactite, stalagmite and white marble in the caves are actually made of calcite.
The main components of the Calhua landscape also include calcite, because the groundwater contains higher HCO 3 - 、Ca 2+ And CO 2 When it emerges from the surface, CO in the environment 2 A sudden decrease in partial pressure, resulting in CO in the water 2 Escape to the atmosphere to form CaCO 3 Deposition, this is called "calsika". The landscape taking the calcium bloom as the main body is a treasure in the nature, and has great humanistic value, scientific research value and economic value. The calcium landscape scenic spots such as the Kyuhaigou and the Huanglonggou attract a large number of tourists to enjoy each year, and become one of the local economic fates. However, the natural calvital landscape has the degradation and damage phenomena of cracking, collapse, corrosion, blackening and the like. Preparation and application research of MinShijie, Dang Zheng Xuan, etc. Ca Hua landscape repairing material [ J]Non-metallic ore 2020(4) 4-7 discloses a method for preparing a calcium bloom block using waste calcium bloom as a raw material, which comprises the steps of carrying out primary crushing on the waste calcium bloom to remove impurities, crushing and sieving the waste calcium bloom by using a jaw crusher and a ball mill, storing the crushed waste calcium bloom block, adding a certain amount of calcium bloom growth promoter and calcium bloom reinforcing agent according to a proportion to prepare a mixture, uniformly stirring the mixture, transferring the mixture into a mould, carrying out compression molding by using a powder tablet press under the pressure of 30MPa, and then carrying out CO compression molding 2 Maintaining for 28 days under the condition for repairing the calcium bloom landscape. However, the preparation process is complex, the cost is high, the preparation time is long, and the production efficiency is low.
In conclusion, the development of a novel method for artificially preparing calcite is of great significance.
Zhangda Da Qin, Jia Zhi just, etc. carbon quantum dot induced calcium carbonate polymorphous particle mineralization and its formation mechanism [ J ] inorganic chemistry report, 2020, 36(8):1557-1566, discloses a method for carbon quantum dot induced calcium carbonate polymorphous particle mineralization, which mainly comprises the steps of preparing carbon quantum dot by heat treatment with citric acid, and then preparing calcium carbonate by induction, however, the cost of citric acid is high.
The invasive plants have very strong growing ability, such as wildfire prairie, which can make people to replace the original plants and destroy the diversity of the local ecosystem. After the successful invasion of most foreign species, the growth vigor of the foreign species is difficult to control, and a single dominant population is formed by suppressing or expelling the native species, so that the ecology of the native species is endangered, and finally, the biodiversity is reduced. The invasive plants have low utilization value and are mainly artificially pulled out or removed by herbicides. The artificial weeding is discarded after weeding, the cost is high, and the influence of the herbicide on the environment is also large. Therefore, the utilization value of the fertilizer is improved, the harm of the fertilizer to the environment is reduced, and economic benefit is brought.
At present, invasive plants are complex in components, and no technology exists for preparing pure calcite from the invasive plants.
Disclosure of Invention
The first problem to be solved by the invention is to provide a method for preparing calcite by inducing herbaceous plants.
In order to solve the first technical problem of the present invention, the method for preparing calcite by herbal induction comprises:
a. preparing the carbon quantum dots: dispersing powder of herbaceous plants in water, reacting for 6-12 h at 200-220 ℃, and carrying out solid-liquid separation to obtain a carbon quantum dot solution, wherein the concentration of the carbon quantum dot solution is 20-25 g/L;
b. preparing calcite: mixing the carbon quantum dot solution and a soluble calcium salt solution to obtain a mixed solution, adding a soluble carbonate solution at a rate of 4-5 mL/min, reacting for 1.9-2.2 h, filtering, washing and drying to obtain calcite;
wherein the herbaceous plant is at least one of alligator alternanthera or aeroponicum praeparatum; the pH value of the carbon quantum dot solution is 6.9-10.35.
The reaction temperature in step a will affect the reaction result, and the reaction temperature is preferably 200-220 ℃.
In one embodiment, the herbal powder has a particle size of 60 mesh or less; the preparation method of the herbaceous plant powder is preferably drying the collected herbaceous plant, cleaning with ethanol and deionized water, drying, grinding, and sieving for later use.
In one embodiment, the powder of the herb plant is dispersed in water and reacted at 210 ℃ for 12 hours in the step a.
In a specific embodiment, the concentration of the carbon quantum dot solution is 22.5 g/L.
In one embodiment, the soluble calcium salt is CaCl 2 、CaBr 2 Or Ca (NO) 3 ) 2 Preferably CaCl, in a mineral oil 2 (ii) a The soluble carbonate Na 2 CO 3 Or K 2 CO 3 Preferably Na 2 CO 3 。
In one embodiment, the concentration of the soluble calcium salt solution is 0.05-0.2 mol/L, preferably 0.1 mol/L; the concentration of the soluble carbonate solution is 0.05-0.2 mol/L, and preferably 0.1 mol/L.
In one embodiment, the volume ratio of the carbon quantum dot solution, the soluble calcium salt solution and the soluble carbonate solution is: 6.75-81: 10-40.
In a specific embodiment, the volume ratio of the carbon quantum dot solution, the soluble calcium salt solution and the soluble carbonate solution is 9:20: 20.
In a specific embodiment, the temperature of the reaction in the step b is 25-29 ℃, and preferably 25 ℃; the reaction time is preferably 2 h; preferably, the reaction in the step b is simultaneously stirred, and the stirring speed is 480-660 r/min.
The second technical problem to be solved by the invention is to provide calcite prepared by inducing herbaceous plants.
In order to solve the second technical problem, the calcite prepared by herbal plant induction is prepared by adopting the method for preparing the calcite by herbal plant induction, the calcite is flower-shaped with a lamellar petal structure, and the petal is preferably square.
Has the advantages that:
(1) by adopting the method, the utilization value of calcite can be improved by preparing calcite from the invasive plants.
(2) The SEM picture of the calcite prepared by the method shows that the calcite has a flower-shaped structure with square petals and is high in purity.
Drawings
FIG. 1 SEM photograph of example 1;
FIG. 2 SEM photograph of example 2;
FIG. 3 SEM photograph of example 4;
FIG. 4 SEM photograph of comparative example 1;
FIG. 5 is an SEM image of comparative example 16;
FIG. 6 is an SEM photograph of comparative example 17;
FIG. 7 is an SEM photograph of comparative example 18;
FIG. 8 is an SEM photograph of comparative example 21;
FIG. 9 is a magenta-producing appearance of calcium carbonate for the examples and some comparative examples;
FIG. 10 is a TG test chart of the calcium carbonate products and the calsiums of examples 1 and 4 and comparative example 25;
FIG. 11 is an XRD pattern of calcium carbonate products of examples 1 and 2 and comparative examples 1-5;
FIG. 12 is an XRD pattern of calcium carbonate products of comparative examples 6-9;
FIG. 13 is an XRD pattern of the calcium carbonate products of comparative examples 10-13;
FIG. 14 is an XRD pattern of the calcium carbonate products of examples 3-7 and comparative examples 22-25;
FIG. 15 XRD patterns of calcium carbonate products of example 1 and comparative examples 18-21;
FIG. 16 is an XRD pattern of calcium carbonate products of example 1 and comparative examples 14-17;
FIG. 17 is a fluorescence diagram of carbon quantum dots of examples and some comparative examples under 455nm excitation.
Detailed Description
In order to solve the first technical problem of the present invention, the method for preparing calcite by inducing herbaceous plants comprises:
a. preparing the carbon quantum dots: dispersing powder of herbaceous plants in water, reacting for 6-12 h at 200-220 ℃, and carrying out solid-liquid separation to obtain a carbon quantum dot solution, wherein the concentration of the carbon quantum dot solution is 20-25 g/L;
b. preparing calcite: mixing the carbon quantum dot solution with a soluble calcium salt solution to obtain a mixed solution, adding a soluble carbonate solution at a rate of 4-5 mL/min, reacting for 1.9-2.2 h, filtering, washing and drying to obtain calcite;
wherein the herbaceous plant is at least one of alligator alternanthera or aeroponicum praeparatum; the pH value of the carbon quantum dot solution is 6.9-10.35.
The reaction temperature in step a will affect the reaction result, and the reaction temperature is preferably 200-220 ℃.
In one embodiment, the herbal powder has a particle size of 60 mesh or less; the preparation method of the herbaceous plant powder is preferably drying the collected herbaceous plant, cleaning with ethanol and deionized water, drying, grinding, and sieving for later use.
In one embodiment, the powder of the herb plant is dispersed in water and reacted at 210 ℃ for 12 hours in the step a.
In a specific embodiment, the concentration of the carbon quantum dot solution is 22.5 g/L.
In one embodiment, the soluble calcium salt is CaCl 2 、CaBr 2 Or Ca (NO) 3 ) 2 Preferably CaCl, in a mineral oil 2 (ii) a The soluble carbonate Na 2 CO 3 Or K 2 CO 3 Preferably Na 2 CO 3 。
In one embodiment, the concentration of the soluble calcium salt solution is 0.05-0.2 mol/L, preferably 0.1 mol/L; the concentration of the soluble carbonate solution is 0.05-0.2 mol/L, and preferably 0.1 mol/L.
In one embodiment, the volume ratio of the carbon quantum dot solution, the soluble calcium salt solution and the soluble carbonate solution is: 6.75-81: 10-40.
In one embodiment, the volume ratio of the carbon quantum dot solution, the soluble calcium salt solution and the soluble carbonate solution is 9:20: 20.
In a specific embodiment, the temperature of the reaction in the step b is 25-29 ℃, and preferably 25 ℃; the reaction time is preferably 2 h; preferably, the reaction in the step b is carried out while stirring, and the stirring speed is 480-660 r/min.
In order to solve the second technical problem, the calcite prepared by herbal plant induction is prepared by adopting the method for preparing the calcite by herbal plant induction, the calcite is in a flower type with a layered petal structure, and preferably, the petals are square.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the invention to the embodiments described.
Example 1
Cleaning glass instruments such as a reaction kettle, a beaker and the like: and (3) primarily brushing and washing the inner container of the reaction kettle and the like by using a test tube brush, adding ethanol into the reaction kettle, ultrasonically washing the reaction kettle for 15min by using an ultrasonic cleaner, taking out the reaction kettle, rinsing the reaction kettle by using deionized water, and drying the reaction kettle at 70 ℃ for later use.
Preparing the carbon quantum dots: drying the collected alligator alternanthera, cleaning the alligator alternanthera with ethanol and deionized water, drying the alligator alternanthera at 70 ℃, grinding the dried alligator alternanthera with a mortar, sieving with a 60-mesh sieve, weighing 0.9g of alligator alternanthera powder sieved by the 60-mesh sieve into a beaker, adding 40mL of ultrapure water into the beaker, stirring with a glass rod, performing ultrasonic dispersion for 5min, pouring the suspension into a reaction kettle, reacting for 12h at 210 ℃, cooling, taking out, performing suction filtration, and sealing and storing the obtained carbon quantum dot solution. Named as CDs-0.9, and the pH is adjusted to 7.35 for standby.
Preparing calcium carbonate: respectively preparing 20mL of 0.1mol/L CaCl in beakers by using deionized water 2 And Na 2 CO 3 Solution 9mL of CDs-0.9 solution was added to CaCl 2 To the solution, mix well with moderate stirring, then add 20mL Na in a constant pressure separatory funnel 2 CO 3 The solution was added to the mixture at a rate of 4.2mL/min and stirred at 550r/min at room temperature (25 ℃) for 2h to complete mineralization. After the reaction is finished, the product is collected by filtration, washed by ultrapure water for many times and dried in an oven at 100 ℃. The prepared sample is preserved and labeled by a sealed bag.
Example 2
The only difference from example 1 is that the herb is aeroponica grass.
Examples 3 to 7
The only difference from example 1 is that the pH is adjusted to: 6.9, 8.35, 8.85, 9.85 and 10.35.
Comparative examples 1 to 13
The only difference from example 1 is that the herbaceous plants are respectively water hyacinth, lantana camara, eupatorium adenophorum, ciliate desert grass, pyroligneous liquor, corn straw, rape straw, wheat straw, rice straw and four humus: four humus are respectively collected at four places of university of Chengdu processing, No. 1 is mixed fallen leaf humus of Sophora heterophylla and tall fescue, fallen leaf humus of bauhinia variegata No. 2, fallen leaf humus of Calonycis 3, mixed humus of Paspalum vaginatum, Rumex acetosa and Sonchus oleraceus 4. The pyroligneous liquor is a reddish brown liquid obtained by condensing and separating a steam gas mixture derived from dry distillation of biomass such as wood in a dry distillation device, and can be self-made or purchased in the market by adopting the prior art. The experiment is to purchase the commercial wood vinegar produced by new energy limited company of Tairan in Shandong.
Comparative examples 14 to 17
The only difference is that 0g, 0.3g, 0.6g and 1.2g of alternanthera philoxeroides powder are respectively weighed in the same way as in example 1.
Comparative examples 18 to 21
The only difference is that the mineralization is completed by moderate stirring at room temperature (25 ℃) for 0.5h, 1h, 4h and 6h, respectively, as in example 1.
Comparative examples 22 to 25
The only difference from example 1 is that the pH is adjusted to: 4.90, 5.35, 5.9, 6.35.
The carbon quantum dots prepared in examples 1 to 7 and comparative examples 1 to 25, and the final calcium carbonate product were subjected to fluorescence detection, infrared detection, TG test, and SEM detection.
It can be seen from the XRD patterns 11-16 that the products produced by the process of the present invention were calcite and that comparative examples 1-24 were mixtures of calcite and vaterite.
It can be seen from SEM images of FIGS. 1-8 that the structures of the products prepared in some examples of the present invention were flower-shaped with square petals, and the structures of the comparative examples were mixed.
As can be seen from the IR image of FIG. 9, the product produced in accordance with the example of the present invention was found to be 711cm -1 、875cm -1 、1420cm -1 Has calcite absorption peak, and other comparative examples are 1087cm -1 And 745cm -1 Has strong absorption peak, the sample has vaterite, and some comparative examples are 1455-1490 cm -1 There is an absorption peak and the sample contains amorphous calcium carbonate.
TG test: n at 100mL/min 2 And (3) performing TG test at the temperature of 0-900 ℃ (the heating rate is 20 ℃/min) in the atmosphere. TG analysis showed that calcium carbonate was decomposed into CaO and CO 2 The temperature range of 560 ℃ to 830 ℃ and the temperature range of 35 ℃ to 330 ℃ for evaporating the water in the ACC particles. See figure 10 for details.
As can be seen from FIG. 17, carbon quantum dot emission of Eupatorium odoratum is similar to that of common water hyacinths and Alternanthera philoxeroides. Other plants have a large deviation from alternanthera philoxeroides.
Claims (19)
1. A method for preparing calcite by herbal induction, the method comprising:
a. preparing the carbon quantum dots: dispersing powder of herbaceous plants in water, reacting for 6-12 h at 200-220 ℃, and carrying out solid-liquid separation to obtain a carbon quantum dot solution, wherein the concentration of the carbon quantum dot solution is 20-25 g/L;
b. preparing calcite: mixing the carbon quantum dot solution and a soluble calcium salt solution to obtain a mixed solution, adding a soluble carbonate solution at a rate of 4-5 mL/min to react for 1.9-2.2 h, filtering, washing and drying to obtain calcite;
wherein the herbaceous plant is at least one of alligator alternanthera or aeroponicum praeparatum; the pH value of the carbon quantum dot solution is 6.9-10.35.
2. The method for the induced production of calcite according to claim 1, wherein the herbaceous plant has a powder size of 60 mesh or less.
3. The method for preparing calcite induced by herbs according to claim 2 wherein the powder of herbs is prepared by drying the collected herbs, washing with ethanol and deionized water, drying, grinding, and sieving.
4. The method for preparing calcite by induction from herbaceous plants as claimed in claim 1, wherein the powder of herbaceous plants is dispersed in water at 210 ℃ for 12h in step a.
5. The method for the induction preparation of calcite according to claim 1 or 2, characterized in that the concentration of the carbon quantum dots solution is 22.5 g/L.
6. The method for the induced production of calcite by herbaceous plants as claimed in claim 1 or 2, characterized in that the soluble calcium salt is CaCl 2 、CaBr 2 Or Ca (NO) 3 ) 2 At least one of; the soluble carbonate Na 2 CO 3 Or K 2 CO 3 At least one of (1).
7. The method of induced preparation of calcite by herbaceous plants as claimed in claim 6, wherein the soluble calcium salt is CaCl 2 。
8. The method for the induced production of calcite by herbaceous plants as claimed in claim 6, characterized in that the soluble carbonate is Na 2 CO 3 。
9. The method for the herbaceous plant induced preparation of calcite according to claim 1 or 2, wherein the concentration of the soluble calcium salt solution is 0.05-0.2 mol/L; the concentration of the soluble carbonate solution is 0.05-0.2 mol/L.
10. The method for the induced production of calcite according to claim 9, wherein the soluble calcium salt solution has a concentration of 0.1 mol/L.
11. The method for the induced production of calcite according to claim 9, characterized in that the concentration of the soluble carbonate solution is 0.1 mol/L.
12. The method for preparing calcite by induction from herbaceous plants according to claim 9, wherein the volume ratio of the carbon quantum dot solution, the soluble calcium salt solution and the soluble carbonate solution is as follows: 6.75-81: 10-40.
13. The method for the induced preparation of calcite according to claim 12, wherein the volume ratio of the carbon quantum dot solution, the soluble calcium salt solution and the soluble carbonate solution is 9:20: 20.
14. The method for preparing calcite by induction from herbaceous plants as claimed in claim 1 or 2, wherein the temperature of the reaction in step b is 25-29 ℃.
15. The process for the induced preparation of calcite according to claim 14, wherein the temperature of the reaction in step b is 25 ℃.
16. The process for the induced production of calcite according to claim 14, characterized in that the reaction time in step b is 2 h.
17. The method for preparing calcite by induction from herbaceous plants as claimed in claim 14, wherein the reaction in step b is carried out with stirring at 480-660 r/min.
18. Herbal plant-induced calcite, which is prepared by the method for preparing calcite through herbal plant induction according to any one of claims 1-17, wherein the calcite is flower-shaped with a layered petal structure.
19. Calcite produced by induction from an herbaceous plant as claimed in claim 18, wherein said petals are square.
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