CN115196663A - Preparation method of controllable nano calcium carbonate - Google Patents
Preparation method of controllable nano calcium carbonate Download PDFInfo
- Publication number
- CN115196663A CN115196663A CN202210944449.8A CN202210944449A CN115196663A CN 115196663 A CN115196663 A CN 115196663A CN 202210944449 A CN202210944449 A CN 202210944449A CN 115196663 A CN115196663 A CN 115196663A
- Authority
- CN
- China
- Prior art keywords
- halogenated
- calcium carbonate
- nano calcium
- imidazole
- amino acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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- 238000002360 preparation method Methods 0.000 title claims description 21
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- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 34
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 34
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- 238000000034 method Methods 0.000 claims abstract description 24
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- 125000000539 amino acid group Chemical group 0.000 claims abstract description 10
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- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 10
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- MTCFGRXMJLQNBG-REOHCLBHSA-N (2S)-2-Amino-3-hydroxypropansäure Chemical compound OC[C@H](N)C(O)=O MTCFGRXMJLQNBG-REOHCLBHSA-N 0.000 claims description 5
- OSSNTDFYBPYIEC-UHFFFAOYSA-N 1-ethenylimidazole Chemical compound C=CN1C=CN=C1 OSSNTDFYBPYIEC-UHFFFAOYSA-N 0.000 claims description 5
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 claims description 5
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- ODKSFYDXXFIFQN-BYPYZUCNSA-P L-argininium(2+) Chemical compound NC(=[NH2+])NCCC[C@H]([NH3+])C(O)=O ODKSFYDXXFIFQN-BYPYZUCNSA-P 0.000 claims description 5
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Abstract
The invention relates to a method for preparing controllable nano calcium carbonate, which comprises the steps of firstly adding disubstituted imidazole type amino acid group ionic liquid into water to prepare a solution of 20 to 60 g/L, and fully stirring; adding a calcium hydroxide suspension to the resulting solution; and then introducing carbon dioxide gas with the content higher than 50% to carry out carbonization reaction to obtain a product, and filtering, washing and drying the product to obtain the dispersed nano calcium carbonate with uniform particle size and the water content lower than 0.1%. The method is simple to operate, green and environment-friendly, and based on the adsorption of the ionic liquid on the surface of the calcium carbonate crystal, the growth rate of crystal nucleus is inhibited, and the agglomeration phenomenon is reduced, so that the nano calcium carbonate particles with good dispersibility are obtained.
Description
Technical Field
The invention relates to the field of inorganic non-metallic materials, in particular to a preparation method of controllable nano calcium carbonate.
Background
Calcium carbonate is an important inorganic carbonate, has the advantages of simple production process, low cost and the like, and is widely applied to the industrial fields of plastics, rubber, coatings, papermaking, medicines and the like. The nano calcium carbonate is an ultrafine solid powder material with the particle size of 1-100 nm, has the characteristics of small particle size, high specific surface area and the like, has reinforcing and modifying effects besides being used as a filler, but the current domestic nano calcium carbonate has wider particle size distribution, is easy to cause agglomeration due to high specific surface energy, has poor compatibility with organic high polymers, and influences the transparency and the dispersibility of the nano calcium carbonate. Therefore, a crystal form control agent, a dispersing agent and the like are usually required to be introduced into a crystallization system, so that the crystal nucleation, the growth rate and the particle morphology are regulated, and the nano calcium carbonate material with narrow particle size distribution and relatively stable product quality and less than 100 nm is prepared.
The ionic liquid is a salt which is composed of organic cations and organic or inorganic anions and is in a liquid state at or near room temperature, has the advantages of environmental friendliness, low surface tension, designable molecular structure, easy formation of hydrogen bonds and the like, and is greatly developed as a good supermolecule structure in inorganic material synthesis in recent years. Furthermore, ionic liquids exhibit high CO 2 Affinity, facilitating the realization of the CO in the gaseous state 2 The enrichment of (2) promotes the formation of calcium carbonate. Meanwhile, the ionic liquid can be adsorbed on the surface of the calcium carbonate crystal to inhibit the growth rate of calcium carbonate crystal nucleus and reduce agglomeration, thereby improving the dispersibility of the nano calcium carbonate particles. Therefore, the synthesis of the nano calcium carbonate with controllable appearance and uniform dispersion is realized by developing the ionic liquid with low cost, stable performance and environmental protectionHas important significance.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of controllable nano calcium carbonate, which is simple to operate and is green and environment-friendly.
In order to solve the problems, the preparation method of the controllable nano calcium carbonate is characterized by comprising the following steps: the method comprises the steps of firstly adding disubstituted imidazole type amino acid group ionic liquid into water to prepare a solution of 20 to 60 g/L, and fully stirring; adding 5 to 10 volume equivalents of calcium hydroxide suspension into the obtained solution, and continuously stirring for 30 to 120 minutes; and then introducing carbon dioxide gas with the content higher than 50% to carry out carbonization reaction, wherein the ventilation rate is 0.1 to 5L/min, the carbonization temperature is 15 to 30 ℃, the stirring speed is 400 to 1000 r/min, the reaction is stopped until the pH value of the suspension is reduced to 6.8 to 8.0, so as to obtain a product, and the product is filtered, washed and dried to obtain the dispersed nano calcium carbonate with uniform particle size and water content lower than 0.1%.
The structural formula of the disubstituted imidazole type amino acid group ionic liquid is as follows:
in the formula: r 1 Is C 1 ~C 8 Alkyl or alkenyl of (a); r 2 Is C 2 ~C 16 Alkyl of (2), or C 2 ~C 16 A hetero carbon chain containing O, or C 1 ~C 14 An amino-containing heterocarbon chain of (a); r 3 Is H or CH 3 (ii) a AA represents amino acid, and is one of glycine, alanine, valine, leucine, isoleucine, phenylalanine, tyrosine, tryptophan, serine, threonine, arginine, histidine, lysine, asparagine, and glutamine.
The disubstituted imidazole type amino acid group ionic liquid is prepared by the following method: firstly, reacting alkyl imidazole or alkenyl imidazole with 1 to 1.2 molar equivalents of halogenated alkane, halogenated alcohol, halogenated ether or halogenated amino halogen acid salt in an organic solvent at 60 to 110 ℃ for 12 to 36 hours, and performing rotary evaporation, washing and drying to obtain a disubstituted imidazolium salt containing halogen anions; then, the obtained ionic salt and 1.1 to 2 molar equivalents of alkali metal hydroxide are stirred and reacted for 2 to 24 hours in an organic solvent at the temperature of 10 to 50 ℃, and a disubstituted imidazolium alkali solution is obtained through filtration, rotary evaporation and drying; and finally reacting the amino acid with a little excessive amino acid in water or absolute ethyl alcohol at room temperature to 60 ℃ for 6 to 24 hours, and performing rotary evaporation, washing and drying to obtain the amino acid.
The alkyl imidazole refers to one of 1-methylimidazole, 1-ethylimidazole, 1-propylimidazole, 1-butylimidazole, 1-pentylimidazole, 1-hexylimidazole, 1-heptylimidazole, 1-octylimidazole, 1, 2-dimethylimidazole, 1-ethyl-2-methylimidazole, 1-propyl-2-methylimidazole and 1-butyl-2-methylimidazole; the alkenyl imidazole is one of 1-vinyl imidazole, 1-allyl imidazole, 2-methyl-1-vinyl imidazole and 1-allyl-2-methyl imidazole; the halogenated alkane refers to one of halogenated ethane, halogenated propane, halogenated isopropane, halogenated butane, halogenated pentane, halogenated hexane, halogenated heptane, halogenated octane, halogenated decane, halogenated dodecane, halogenated tetradecane and halogenated hexadecane; the halogenated alcohol is one of 2-halogenated ethanol, 3-halogenated-1-propanol, 4-halogenated-1-butanol, 1-halogenated-2-butanol, 5-halogenated-1-pentanol, 6-halogenated-1-hexanol, 7-halogenated-1-heptanol, 8-halogenated-1-octanol, 9-halogenated-1-nonanol, 10-halogenated-1-decanol, 12-halogenated-1-dodecanol, 14-halogenated-1-tetradecanol and 16-halogenated-1-hexadecanol; the halogenated ether is one of 1-halogenated-2-methoxyethane, 1-halogenated-3-methoxypropane, 1-halogenated-4-methoxybutane, 1-halogenated-2-ethoxyethane, 2-halogenated-1, 1-diethoxyethane and 1-halogenated-2, 2-dimethoxypropane; the halogenated amino hydrohalide is one of 2-halogenated ethylamine halide, 3-halogenated propylamine halide, bis (2-halogenated ethyl) amine halide, N- (2-halogenated ethyl) -1, 3-propanediamine dihydrohalide, N-dimethyl-2-halogenated propylamine halide, 2-halogenated triethylamine halide, 2-halogenated propanediamine halide and 2-chloropropanediamine hydrochloride; the alkali metal hydroxide refers to one of sodium hydroxide and potassium hydroxide.
The concentration of the calcium hydroxide suspension is 80-130 g/L, and the calcium hydroxide suspension is prepared by adding quick lime into hot water of 40-90 ℃ and stirring and digesting for 30-120 minutes, or by directly adding raw material calcium hydroxide into water for preparation.
The carbonization process utilizes circulating cooling water to control the temperature difference of a reaction system within the range of +/-2 ℃.
The drying temperature is 100 to 200 ℃, and the drying time is 2 to 6 hours.
The particle size of the nano calcium carbonate is 10 to 100 nm, and the morphology is one of cube, sphere, spindle and chain.
Compared with the prior art, the invention has the following advantages:
1. the invention takes disubstituted imidazole type amino acid group ionic liquid as a template agent, and obtains the nano calcium carbonate material with specific morphology and uniform grain diameter by regulating and controlling the nucleation and growth rate of the crystal and the dispersity in a solvent based on the adsorption of the ionic liquid on the surface of the calcium carbonate crystal.
2. The invention prepares the nano calcium carbonate with different particle sizes and appearances by changing the type and concentration of the ionic liquid, and can meet the requirements of different fields on the nano calcium carbonate.
3. The method is simple to operate, low in cost and environment-friendly.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is an SEM photograph of nano calcium carbonate in example 1 of the present invention.
FIG. 2 is a nuclear magnetic hydrogen spectrum characterization of the ionic liquid in example 1 of the present invention.
Detailed Description
A controllable nano calcium carbonate preparation method is that a disubstituted imidazole amino acid base ionic liquid is added into water to prepare a solution with the concentration of 20 to 60 g/L, and the solution is fully stirred; adding 5 to 10 volume equivalents of calcium hydroxide suspension into the obtained solution, and continuously stirring for 30 to 120 minutes; and then introducing carbon dioxide gas with the content higher than 50% to carry out carbonization reaction, wherein the aeration rate is 0.1 to 5L/min, the carbonization temperature is 15 to 30 ℃, the stirring speed is 400 to 1000 r/min, and the reaction is stopped until the pH value of the suspension is reduced to 6.8 to 8.0. The temperature difference of the reaction system is controlled within the range of +/-2 ℃ by using circulating cooling water in the carbonization process. And (3) obtaining a product after the reaction is finished, filtering the product, washing the product by using deionized water or a deionized water-ethanol mixed solution, and drying the product for 2 to 6 hours at the temperature of 100 to 200 ℃ to obtain the dispersed nano calcium carbonate with uniform particle size and the water content of less than 0.1%. The particle size of the nano calcium carbonate is 10 to 100 nm, and the morphology is one of cube, sphere, spindle and chain.
Wherein: the structural formula of the disubstituted imidazole type amino acid group ionic liquid is as follows:
in the formula: r is 1 Is C 1 ~C 8 Alkyl or alkenyl of (a); r is 2 Is C 2 ~C 16 Alkyl of (a), or C 2 ~C 16 A hetero carbon chain containing O, or C 1 ~C 14 An amino-containing heterocarbon chain of (a); r 3 Is H or CH 3 (ii) a AA represents amino acid, and is one of glycine, alanine, valine, leucine, isoleucine, phenylalanine, leucine, tryptophan, serine, threonine, arginine, histidine, lysine, asparagine, and glutamine.
The disubstituted imidazole type amino acid group ionic liquid is prepared by the following method: firstly, alkyl imidazole or alkenyl imidazole reacts with 1 to 1.2 molar equivalents of halogenated alkane, halogenated alcohol, halogenated ether or halogenated amino hydrogen halide in an organic solvent such as acetonitrile, ethyl acetate, acetone and the like at 60 to 110 ℃ for 12 to 36 hours, is subjected to rotary evaporation at 40 to 80 ℃ for 0.2 to 1 hour, is washed by diethyl ether, ethanol, ethyl acetate or tetrahydrofuran and is dried at 50 to 80 ℃ for 4 to 12 hours to obtain a disubstituted imidazolium salt containing halogen anions; then, the obtained ionic salt and 1.1 to 2 molar equivalents of alkali metal hydroxide are stirred and reacted for 2 to 24 hours at 10 to 50 ℃ in an organic solvent such as deionized water, ethanol, acetonitrile, acetone and the like, the obtained ionic salt is filtered, rotary-evaporated for 0.2 to 1 hour at 40 to 80 ℃, and then dried for 4 to 12 hours at 50 to 80 ℃ to obtain a disubstituted imidazolium alkali solution; and finally reacting the amino acid with a little excessive amino acid in water or absolute ethyl alcohol at room temperature to 60 ℃ for 6 to 24 hours, filtering, carrying out rotary evaporation at 50 to 95 ℃ for 0.2 to 1.5 hours, washing with water or absolute ethyl alcohol, and drying at 50 to 95 ℃ for 4 to 12 hours to obtain the amino acid.
The alkyl imidazole is one of 1-methylimidazole, 1-ethylimidazole, 1-propylimidazole, 1-butylimidazole, 1-pentylimidazole, 1-hexylimidazole, 1-heptylimidazole, 1-octylimidazole, 1, 2-dimethylimidazole, 1-ethyl-2-methylimidazole, 1-propyl-2-methylimidazole and 1-butyl-2-methylimidazole.
The alkenyl imidazole is one of 1-vinyl imidazole, 1-allyl imidazole, 2-methyl-1-vinyl imidazole and 1-allyl-2-methyl imidazole.
The halogenated alkane refers to one of halogenated ethane, halogenated propane, halogenated isopropane, halogenated butane, halogenated pentane, halogenated hexane, halogenated heptane, halogenated octane, halogenated decane, halogenated dodecane, halogenated tetradecane and halogenated hexadecane.
The halogenated alcohol is one of 2-halogenated ethanol, 3-halogenated-1-propanol, 4-halogenated-1-butanol, 1-halogenated-2-butanol, 5-halogenated-1-pentanol, 6-halogenated-1-hexanol, 7-halogenated-1-heptanol, 8-halogenated-1-octanol, 9-halogenated-1-nonanol, 10-halogenated-1-decanol, 12-halogenated-1-dodecanol, 14-halogenated-1-tetradecanol and 16-halogenated-1-hexadecanol.
The halogenated ether is one of 1-halogenated-2-methoxyethane, 1-halogenated-3-methoxypropane, 1-halogenated-4-methoxybutane, 1-halogenated-2-ethoxyethane, 2-halogenated-1, 1-diethoxyethane and 1-halogenated-2, 2-dimethoxypropane.
The halogenated amino hydrohalide is one of 2-halogenated ethylamine halide, 3-halogenated propylamine halide, bis (2-haloethyl) amine halide, N- (2-haloethyl) -1, 3-propanediamine dihydrohalide, N-dimethyl-2-halogenated propylamine halide, 2-halogenated triethylamine halide, 2-halogenated propanediamine halide and 2-chloropropanediamine hydrochloride (CAS number: 55526-63-1); halogen is preferably chlorine and bromine.
The alkali metal hydroxide is one of sodium hydroxide and potassium hydroxide.
The concentration of the calcium hydroxide suspension is 80 to 130 g/L, and the calcium hydroxide suspension is prepared by adding quicklime into hot water with the temperature of 40 to 90 ℃, stirring and digesting for 30 to 120 minutes, or is prepared by directly adding raw material calcium hydroxide into water.
Embodiment 1A controllable nanometer calcium carbonate preparation method, said method comprises adding 1-aminoethyl-3-methylimidazole glycinate ionic liquid to make 30 g/L solution in water first, and fully stirring; adding 5 volume equivalents of calcium hydroxide suspension into the obtained solution, and continuing stirring for 60 minutes; and then introducing carbon dioxide gas with the content higher than 50% to carry out carbonization reaction, wherein the aeration rate is 1L/min, the carbonization temperature is 18 +/-2 ℃, the stirring speed is 500 rpm, and the reaction is stopped until the pH value of the suspension is reduced to 7-7.5. And (3) obtaining a product after the reaction is finished, filtering the product, washing the product by using deionized water, and drying the product at 110 ℃ for 6 hours to obtain the dispersed cubic nano calcium carbonate with the particle size of 30 to 50 nm, wherein the dispersed cubic nano calcium carbonate is shown in a figure 1.
Wherein: the structural formula of the 1-aminoethyl-3-methylimidazole glycinate ionic liquid is as follows:
the preparation method comprises the following steps:
firstly, 1-methylimidazole reacts with 1.1 molar equivalent of 2-bromoethylamine hydrobromide in acetonitrile at 70 ℃ for 24 hours, 1.2 molar equivalent of sodium hydroxide is added, stirring is carried out, and then the mixture is subjected to rotary evaporation at 70 ℃, washing by ethanol-tetrahydrofuran (V: V = 1) and drying at 60 ℃ for 6 hours to obtain 1-aminoethyl-3-methylimidazole bromide ionic liquid; then stirring the obtained ionic salt and 1.2 molar equivalents of sodium hydroxide in deionized water at 25 ℃ for 6 hours, and filtering, rotary steaming and drying to obtain 1-aminoethyl-3-methylimidazolium hydroxide; finally reacting with 1.05 molar equivalent of glycine in deionized water at room temperature for 24 hours, filtering, carrying out rotary evaporation at 80 ℃, washing with deionized water, and drying at 85 ℃ to obtain the product.
For the obtained 1-aminopropyl-3-methylimidazolium glycinate ionic liquidThe body was subjected to nuclear magnetic hydrogen spectroscopy, as shown in figure 2. 1 H NMR（400 MHz，DMSO-d 6 ）δ：9.79（s，1H，N＝CH—N），7.81（s，1H，CH＝CH），7.76（s，1H，CH＝CH），4.20（t，J＝ 5.8 Hz，2H，—CH 2 —CH 2 ），3.87（s，3H，—CH 3 ），2.87（dd，J＝ 12.5，6.8 Hz，2H，—CH 2 —CH 2 ），2.75（s，2H， - OOC—CH 2 ). In conclusion, it can be seen that glycine is successfully introduced into imidazole groups in the ionic liquid.
The calcium hydroxide suspension is prepared by adding quicklime into hot water of 40 ℃, stirring and digesting for 60 minutes, and the concentration of the calcium hydroxide suspension is 100 g/L.
Embodiment 2A controllable nanometer calcium carbonate preparation method, this method means that add 1-dodecyl-3-methylimidazole arginine salt ionic liquid to make 35 g/L solution in water first, and fully stir; adding 5 volume equivalents of calcium hydroxide suspension into the obtained solution, and continuing stirring for 60 minutes; and then introducing carbon dioxide gas with the content higher than 50% to carry out carbonization reaction, wherein the aeration rate is 2.8L/min, the carbonization temperature is 25 +/-2 ℃, the stirring speed is 800 r/min, and the reaction is stopped until the pH value of the suspension is reduced to 7.2-7.8. And (3) obtaining a product after the reaction is finished, filtering the product, washing the product by using a deionized water-ethanol (V: V = 9).
Wherein: the structural formula of the 1-dodecyl-3-methylimidazole arginine salt ionic liquid is as follows:
the preparation method comprises the following steps:
firstly, 1-methylimidazole reacts with 1.1 molar equivalent of 1-chlorododecane in acetonitrile at 60 ℃ for 12 hours, and then the 1-dodecyl-3-methylimidazole chloride ionic liquid is obtained after rotary evaporation at 70 ℃, ether washing and drying at 50 ℃ for 6 hours; then stirring the obtained ionic salt and 1.1 molar equivalent of sodium hydroxide in deionized water at 30 ℃ for 6 hours, filtering, rotary evaporating and drying to obtain 1-dodecyl-3-methylimidazolium hydroxide; finally reacting with 1.1 molar equivalent of arginine in deionized water at 40 ℃ for 18 hours, filtering, carrying out rotary evaporation at 80 ℃, washing with deionized water, and drying at 85 ℃ to obtain the arginine-containing chitosan.
The calcium hydroxide suspension is prepared by directly adding raw material calcium hydroxide into water, and the concentration of the calcium hydroxide suspension is 120 g/L.
Embodiment 3A controllable nanometer calcium carbonate preparation method, this method means that add 1-methoxy ethyl-2-methyl-3-ethyl imidazole alanine salt ionic liquid to make 50 g/L solution in water first, and fully stir; adding a calcium hydroxide suspension with 8 volume equivalents into the obtained solution, and continuously stirring for 30 to 120 minutes; and then introducing carbon dioxide gas with the content higher than 50% to carry out carbonization reaction, wherein the aeration rate is 1.2L/min, the carbonization temperature is 28 +/-2 ℃, the stirring speed is 500 rpm, and the reaction is stopped until the pH value of the suspension is reduced to 7.5-8.0. And (3) obtaining a product after the reaction is finished, filtering the product, washing the product by using deionized water, and drying the product at 130 ℃ for 4 hours to obtain the dispersed spherical nano calcium carbonate with the particle size of 40 to 60 nm.
Wherein: the structural formula of the 1-methoxyethyl-2-methyl-3-ethylimidazole alanine salt ionic liquid is as follows:
the preparation method comprises the following steps:
firstly, 1-ethyl-2-methylimidazole reacts with 1.05 molar equivalent of 1-chloro-2-methoxyethane in ethyl acetate at 60 ℃ for 12 hours, and then the 1-methoxyethyl-2-methyl-3-ethylimidazole chloride ionic liquid is obtained after rotary evaporation at 60 ℃, ether washing and drying at 50 ℃ for 6 hours; then the obtained ionic salt and 1.1 molar equivalent of sodium hydroxide are stirred and reacted for 12 hours at 40 ℃ in deionized water, and 1-methoxyethyl-2-methyl-3-ethylimidazolium hydroxide is obtained through filtration, rotary evaporation and drying; finally reacting with 1.1 molar equivalent of alanine salt in absolute ethyl alcohol at 40 ℃ for 12 hours, filtering, carrying out rotary evaporation at 50 ℃, washing with absolute ethyl alcohol, and drying at 70 ℃ to obtain the product.
The calcium hydroxide suspension is prepared by directly adding raw material calcium hydroxide into water, and the concentration of the calcium hydroxide suspension is 90 g/L.
Embodiment 4A controllable nanometer calcium carbonate preparation method, said method comprises adding 1-vinyl-3-butyl imidazole isoleucine salt ionic liquid to prepare 60 g/L solution in water first, and fully stir; adding 9 volume equivalents of calcium hydroxide suspension into the obtained solution, and continuing stirring for 80 minutes; and then introducing 80% carbon dioxide gas for carbonization reaction, wherein the aeration rate is 2.0L/min, the carbonization temperature is 18 +/-2 ℃, the stirring speed is 600 r/min, and the reaction is stopped until the pH value of the suspension is reduced to 6.8-7.2. And (3) obtaining a product after the reaction is finished, filtering the product, washing the product by using deionized water-ethanol (V: V = 8).
Wherein: the structural formula of the 1-vinyl-3-butylimidazole isoleucine salt ionic liquid is as follows:
the preparation method comprises the following steps:
firstly, 1-vinyl imidazole reacts with 1.02 molar equivalent of 1-bromobutane in acetone for 24 hours at 80 ℃, and then 1-vinyl-3-butyl imidazole bromide ionic liquid is obtained after rotary evaporation at 80 ℃, ethyl acetate washing and drying at 60 ℃ for 6 hours; then stirring the obtained ionic salt and 1.02 molar equivalent of sodium hydroxide in deionized water at 40 ℃ for 6 hours to react, and filtering, rotary steaming and drying to obtain 1-vinyl-3-butylimidazolium hydroxide; finally reacting with 1.1 molar equivalent of isoleucine in water at 50 ℃ for 24 hours, filtering, carrying out rotary evaporation at 85 ℃, washing with deionized water, and drying at 90 ℃ to obtain the final product.
The calcium hydroxide suspension is prepared by adding quicklime into hot water of 50 ℃, stirring and digesting for 80 minutes, and the concentration of the calcium hydroxide suspension is 120 g/L.
Embodiment 5A controllable nanometer calcium carbonate preparation method, said method comprises adding 1-hydroxyethyl-3-vinyl imidazole serine ionic liquid to make 48 g/L solution in water first, and fully stir; adding 10 volume equivalents of calcium hydroxide suspension to the obtained solution, and continuing stirring for 60 minutes; then carbon dioxide gas with the content of 90% is introduced for carbonization reaction, the aeration rate is 1.5L/min, the carbonization temperature is 20 +/-2 ℃, the stirring speed is 600 rpm, and the reaction is stopped until the pH value of the suspension is reduced to 7.5-8.0. And (3) obtaining a product after the reaction is finished, filtering the product, washing the product by using deionized water-ethanol (V: V = 9).
Wherein: the structural formula of the 1-hydroxyethyl-3-vinyl imidazole serine ionic liquid is as follows:
the preparation method comprises the following steps:
firstly, 1-vinyl imidazole reacts with 1.1 molar equivalent of 2-bromoethanol in acetone at 70 ℃ for 12 hours, and then 1-hydroxyethyl-3-vinyl imidazole bromide ionic liquid is obtained after rotary evaporation at 70 ℃, ethyl acetate washing and drying at 70 ℃ for 6 hours; then the obtained ionic salt and 1.05 molar equivalent of potassium hydroxide are stirred and reacted for 6 hours at 40 ℃ in deionized water, and the 1-hydroxyethyl-3-vinyl imidazolium hydroxide is obtained through filtration, rotary evaporation and drying; and finally reacting with 1.1 molar equivalent of serine in deionized water at room temperature for 24 hours, filtering, carrying out rotary evaporation at 85 ℃, washing with deionized water, and drying at 90 ℃ to obtain the serine.
The calcium hydroxide suspension is prepared by directly adding raw material calcium hydroxide into water, and the concentration of the calcium hydroxide suspension is 100 g/L.
Embodiment 6A controllable nanometer calcium carbonate preparation method, the method means that add 1-amine propyl-3-propyl imidazole histidine salt ionic liquid to prepare 50 g/L solution in water first, and fully stir; adding 8 volume equivalents of calcium hydroxide suspension to the obtained solution, and continuing stirring for 60 minutes; and then introducing carbon dioxide gas with the content higher than 50% to carry out carbonization reaction, wherein the aeration rate is 1.8L/min, the carbonization temperature is 25 +/-2 ℃, the stirring speed is 800 r/min, and the reaction is stopped until the pH value of the suspension is reduced to 7.0-7.5. And (3) obtaining a product after the reaction is finished, filtering the product, washing the product by using deionized water-ethanol (V: V = 7).
Wherein: the structural formula of the 1-aminopropyl-3-propylimidazolium salt ionic liquid is as follows:
the preparation method comprises the following steps:
firstly, 1-propylimidazole reacts with 1.1 molar equivalent of 3-bromopropylamine hydrobromide in tetrahydrofuran at 80 ℃ for 24 hours, 1.1 molar equivalent of potassium hydroxide is added, stirred, subjected to rotary evaporation at 80 ℃, washed by ethanol-tetrahydrofuran (V: V = 1), and dried at 50 ℃ for 6 hours to obtain 1-aminopropyl-3-propylimidazole bromide ionic liquid; then stirring the obtained ionic salt and 1.1 molar equivalent of potassium hydroxide in deionized water at 40 ℃ for 6 hours to react, and obtaining 1-aminopropyl-3-propylimidazolium hydroxide through filtration, rotary evaporation and drying; finally reacting with 1.1 molar equivalent of histidine in deionized water at 40 ℃ for 20 hours, filtering, carrying out rotary evaporation at 80 ℃, washing with deionized water, and drying at 85 ℃ to obtain the final product.
The calcium hydroxide suspension is prepared by adding quicklime into hot water of 60 ℃ and stirring and digesting for 60 minutes, and the concentration of the calcium hydroxide suspension is 125 g/L.
It is to be understood that the embodiments discussed herein are for illustrative purposes only and that various modifications or changes in light thereof will be suggested to persons skilled in the art and are to be included within the spirit and purview of this application and scope of the appended claims.
Claims (8)
1. A preparation method of controllable nano calcium carbonate is characterized by comprising the following steps: the method comprises the steps of firstly adding disubstituted imidazole type amino acid group ionic liquid into water to prepare a solution of 20 to 60 g/L, and fully stirring; adding 5 to 10 volume equivalents of calcium hydroxide suspension into the obtained solution, and continuously stirring for 30 to 120 minutes; and then introducing carbon dioxide gas with the content higher than 50% to carry out carbonization reaction, wherein the ventilation rate is 0.1 to 5L/min, the carbonization temperature is 15 to 30 ℃, the stirring speed is 400 to 1000 r/min, the reaction is stopped until the pH value of the suspension is reduced to 6.8 to 8.0, so as to obtain a product, and the product is filtered, washed and dried to obtain the dispersed nano calcium carbonate with uniform particle size and water content lower than 0.1%.
2. The method for preparing controllable nano calcium carbonate according to claim 1, which is characterized in that: the structural formula of the disubstituted imidazole type amino acid group ionic liquid is as follows:
in the formula: r 1 Is C 1 ~C 8 Alkyl or alkenyl of (a); r is 2 Is C 2 ~C 16 Alkyl of (2), or C 2 ~C 16 A hetero carbon chain containing O, or C 1 ~C 14 An amino-containing heterocarbon chain of (a); r 3 Is H or CH 3 (ii) a AA represents amino acid, and is one of glycine, alanine, valine, leucine, isoleucine, phenylalanine, leucine, tryptophan, serine, threonine, arginine, histidine, lysine, asparagine, and glutamine.
3. The method for preparing controllable nano calcium carbonate according to claim 2, which is characterized by comprising the following steps: the disubstituted imidazole type amino acid group ionic liquid is prepared by the following method: firstly, alkyl imidazole or alkenyl imidazole reacts with 1 to 1.2 molar equivalents of halogenated alkane, halogenated alcohol, halogenated ether or halogenated amino halogen acid salt in an organic solvent at 60 to 110 ℃ for 12 to 36 hours, and the disubstituted imidazolium salt containing halogen anions is obtained through rotary evaporation, washing and drying; then, the obtained ionic salt and 1.1 to 2 molar equivalents of alkali metal hydroxide are stirred and reacted for 2 to 24 hours in an organic solvent at the temperature of 10 to 50 ℃, and a disubstituted imidazolium alkali solution is obtained through filtration, rotary evaporation and drying; and finally reacting the amino acid with a little excessive amino acid in water or absolute ethyl alcohol at room temperature to 60 ℃ for 6 to 24 hours, and performing rotary evaporation, washing and drying to obtain the amino acid.
4. The method for preparing controllable nano calcium carbonate according to claim 3, which is characterized in that: the alkyl imidazole refers to one of 1-methylimidazole, 1-ethylimidazole, 1-propylimidazole, 1-butylimidazole, 1-pentylimidazole, 1-hexylimidazole, 1-heptylimidazole, 1-octylimidazole, 1, 2-dimethylimidazole, 1-ethyl-2-methylimidazole, 1-propyl-2-methylimidazole and 1-butyl-2-methylimidazole; the alkenyl imidazole is one of 1-vinyl imidazole, 1-allyl imidazole, 2-methyl-1-vinyl imidazole and 1-allyl-2-methyl imidazole; the halogenated alkane refers to one of halogenated ethane, halogenated propane, halogenated isopropane, halogenated butane, halogenated pentane, halogenated hexane, halogenated heptane, halogenated octane, halogenated decane, halogenated dodecane, halogenated tetradecane and halogenated hexadecane; the halogenated alcohol is one of 2-halogenated ethanol, 3-halogenated-1-propanol, 4-halogenated-1-butanol, 1-halogenated-2-butanol, 5-halogenated-1-pentanol, 6-halogenated-1-hexanol, 7-halogenated-1-heptanol, 8-halogenated-1-octanol, 9-halogenated-1-nonanol, 10-halogenated-1-decanol, 12-halogenated-1-dodecanol, 14-halogenated-1-tetradecanol and 16-halogenated-1-hexadecanol; the halogenated ether is one of 1-halogenated-2-methoxyethane, 1-halogenated-3-methoxypropane, 1-halogenated-4-methoxybutane, 1-halogenated-2-ethoxyethane, 2-halogenated-1, 1-diethoxyethane and 1-halogenated-2, 2-dimethoxypropane; the halogenated amino hydrohalide is one of 2-halogenated ethylamine halide, 3-halogenated propylamine halide, bis (2-halogenated ethyl) amine halide, N- (2-halogenated ethyl) -1, 3-propanediamine dihydrohalide, N-dimethyl-2-halogenated propylamine halide, 2-halogenated triethylamine halide, 2-halogenated propanediamine halide and 2-chloropropanediamine hydrochloride; the alkali metal hydroxide refers to one of sodium hydroxide and potassium hydroxide.
5. The method for preparing controllable nano calcium carbonate according to claim 1, which is characterized in that: the concentration of the calcium hydroxide suspension is 80-130 g/L, and the calcium hydroxide suspension is prepared by adding quick lime into hot water of 40-90 ℃ and stirring and digesting for 30-120 minutes, or by directly adding raw material calcium hydroxide into water for preparation.
6. The method for preparing controllable nano calcium carbonate according to claim 1, which is characterized in that: the carbonization process utilizes circulating cooling water to control the temperature difference of a reaction system within the range of +/-2 ℃.
7. The method for preparing controllable nano calcium carbonate according to claim 1, which is characterized in that: the drying temperature is 100 to 200 ℃, and the drying time is 2 to 6 hours.
8. The method for preparing controllable nano calcium carbonate according to claim 1, which is characterized in that: the particle size of the nano calcium carbonate is 10-100 nm, and the shape of the nano calcium carbonate is one of a cube, a sphere, a spindle and a chain.
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