CN116731392A - Calcium carbonate composite material with ultraviolet shielding performance and preparation method thereof - Google Patents
Calcium carbonate composite material with ultraviolet shielding performance and preparation method thereof Download PDFInfo
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- CN116731392A CN116731392A CN202310730378.6A CN202310730378A CN116731392A CN 116731392 A CN116731392 A CN 116731392A CN 202310730378 A CN202310730378 A CN 202310730378A CN 116731392 A CN116731392 A CN 116731392A
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- ultraviolet shielding
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- calcium carbonate
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 70
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 19
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000654 additive Substances 0.000 claims abstract description 8
- 230000000996 additive effect Effects 0.000 claims abstract description 8
- 230000015556 catabolic process Effects 0.000 claims abstract description 4
- 238000006731 degradation reaction Methods 0.000 claims abstract description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 4
- 230000003197 catalytic effect Effects 0.000 claims abstract description 3
- 238000005260 corrosion Methods 0.000 claims abstract 2
- 230000007797 corrosion Effects 0.000 claims abstract 2
- 239000002096 quantum dot Substances 0.000 claims abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 229940082328 manganese acetate tetrahydrate Drugs 0.000 claims description 8
- CESXSDZNZGSWSP-UHFFFAOYSA-L manganese(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Mn+2].CC([O-])=O.CC([O-])=O CESXSDZNZGSWSP-UHFFFAOYSA-L 0.000 claims description 8
- -1 polyoxyethylene lauryl ether Polymers 0.000 claims description 8
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 7
- 239000012498 ultrapure water Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000004729 solvothermal method Methods 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 claims 1
- 239000002105 nanoparticle Substances 0.000 abstract description 6
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052748 manganese Inorganic materials 0.000 abstract description 3
- 239000011572 manganese Substances 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 239000002667 nucleating agent Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 239000011575 calcium Substances 0.000 abstract 1
- 238000000975 co-precipitation Methods 0.000 abstract 1
- 238000013329 compounding Methods 0.000 abstract 1
- 239000004800 polyvinyl chloride Substances 0.000 description 23
- 229920000915 polyvinyl chloride Polymers 0.000 description 22
- 229920003023 plastic Polymers 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000000411 transmission spectrum Methods 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a calcium carbonate composite material with ultraviolet shielding performance and a preparation method thereof, wherein manganese doped carbon quantum dots (Mn-CDs) react with tetraethoxysilane in a microemulsion system in a completely dispersed state to prepare Mn-CDs@SiO 2 Nanoparticles using Mn-CDs and SiO 2 The synergistic effect of the (2) improves the ultraviolet shielding capability of the nano particles and simultaneously controls the particle size of the nucleating agent. Mn-CDs@SiO is prepared by a simple coprecipitation method 2 At room temperature with calcium carbonate (CaCO) 3 ) Compounding to prepare environment-friendly Ca with ultraviolet shielding performanceCO 3 Composite material (Mn-CDs@SiO) 2 @CaCO 3 ). The invention has simple steps, strong operability and CaCO 3 Free radicals are not generated when the base material is irradiated or heated, and the base material has excellent corrosion resistance and heat resistance, and can effectively avoid photo (thermal) catalytic degradation of the base material. Prepared CaCO 3 The composite material has excellent ultraviolet shielding performance and endows PVC with CaCO as a common additive 3 The novel performance is an innovative application of the inorganic quantum dots, expands CaCO 3 The ultraviolet shielding additive can be used as an ultraviolet shielding additive in PVC materials in outdoor or special places in the application range of the PVC and other material fields.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a calcium carbonate composite material with ultraviolet shielding performance and a preparation method thereof.
Background
Polyvinyl chloride (PVC) is widely used in many fields as one of general plastics, because of its excellent chemical stability, abrasion resistance, electrical insulation, water resistance, tensile/compressive properties, low price, and mature production process. However, the ultraviolet light resistance and the thermal stability are poor, the ultraviolet light resistance and the thermal stability can be influenced by various external environmental factors when the ultraviolet light resistance type ultraviolet light-sensitive material is used in an outdoor environment or in some special occasions, and particularly the ultraviolet light resistance type ultraviolet light-sensitive material can be photodegradation, so that the appearance and physical and chemical properties of the material are promoted to be changed.
Calcium carbonate (CaCO) 3 ) Is a functional material developed in the 80 s of the 20 th century, does not generate free radicals and can effectively avoid the degradation of PVC under the photo-thermal condition. As an important inorganic filler in PVC pipe processing, calcium carbonate not only can improve the strength, toughness, heat resistance, dimensional stability and other performance indexes of a pipeline product, but also can replace expensive white pigment to play a certain whitening role, but also can be used as filler CaCO 3 But the ultraviolet shielding ability of (c) is poor.
CN201610247632.7 discloses a CaCO for PVC 3 The CaCO prepared by the method 3 The PVC plastic has good compatibility with PVC resin, can obviously improve the mechanical property of PVC plastic after filling, and can also effectively avoid the adverse effect of iron ions on the gloss of PVC.
The inorganic ultraviolet screening agent commonly used at present achieves the purpose of screening ultraviolet mainly through reflecting or refracting ultraviolet, and has the advantages of no toxicity, no smell, no irritation, chemical stability and the like.
In combination with the advantages of improving the comprehensive performance of the PVC substrate by utilizing the calcium carbonate, caCO with good ultraviolet shielding performance, low cost, simplicity and easy operation is developed 3 The composite material has important significance for expanding the application field of PVC materials.
In order to achieve the aim, the invention firstly introduces SiO with ultraviolet shielding function on the surface of the manganese doped carbon quantum dot with strong ultraviolet shielding performance 2 By Mn-CDs and SiO 2 Synergistic effect elevation of (2)The ultraviolet shielding capability of the nano particles, the particle size of the nucleating agent is controlled, and then CaCO is wrapped 3 Obtaining the calcium carbonate composite material with excellent ultraviolet shielding performance, and is hopeful to further expand the functional material CaCO 3 Is used in the application range of (a).
Disclosure of Invention
The invention provides a modified calcium carbonate which aims at overcoming the defect of poor ultraviolet shielding capability of the calcium carbonate in the prior art and comprises Mn-CDs and tetraethoxysilane for CaCO 3 The ultraviolet shielding agent is prepared by functionalization and can be used as a filler to optimize the comprehensive performance of PVC.
The invention adopts the following specific technical scheme for realizing the purpose:
1. dissolving manganese acetate tetrahydrate and o-phenylenediamine in absolute ethyl alcohol, carrying out solvothermal reaction for 12 hours at 180 ℃, centrifuging, washing and drying to obtain manganese doped carbon quantum dots (Mn-CDs).
2. Mn-CDs, heptane and polyoxyethylene lauryl ether are stirred and mixed uniformly, ultrapure water and concentrated ammonia water are dripped into the mixture, tetraethoxysilane (TEOS) is added after stirring for 1h, the reaction is continued for 72h under stirring at room temperature, ethanol is added to lead the microemulsion to be completely precipitated, and Mn-CDs@SiO is obtained after centrifugation, washing and drying 2 。
3、Mn-CDs@SiO 2 Dissolving in CaCl 2 Stirring and mixing the solution uniformly, and rapidly adding Na 2 CO 3 The solution is reacted for 24 hours at room temperature under 1000rpm magnetic stirring, and is centrifuged, washed and dried to obtain Mn-CDs@SiO 2 @CaCO 3 。
Preferably, the test water is self-made ultrapure water.
Preferably, the ratio of the mass of manganese acetate tetrahydrate to that of o-phenylenediamine in scheme 1 = 6g:1g.
Preferably, the molar volume ratio of manganese acetate tetrahydrate to absolute ethanol in scheme 1 = 1mmol: (10-12) mL.
Preferably, in scheme 2, the mass to volume ratio of Mn-CDs, heptane, polyoxyethylene lauryl ether=1g: (35-40) mL: (10-15) mL, volume ratio of heptane and ultrapure water, concentrated ammonia water = 1mL:0.05mL:0.01ml, mass to volume ratio of mn-CD and ethyl orthosilicate = 1g: (1.0-1.2) mL.
Preferably, caCl in scheme 3 2 And Na (Na) 2 CO 3 Volume ratio of solution = 1:1, the concentration of the two is 0.1mol/L, mn-CDs@SiO 2 And CaCl 2 Mass volume ratio of solution= (0.01-0.02) g:1mL of the solution was used for the treatment of the waste heat,
preferably, the washing in each step is carried out by washing with deionized water and then washing with absolute ethanol.
Preferably, the drying temperature in schemes 1, 2 and 3 is 60 to 70 ℃.
The method has simple steps and strong operability, and endows the PVC with CaCO which is a common additive 3 The PVC material has new performance, no ultraviolet light or thermal catalytic degradation activity, excellent ultraviolet shielding performance, and can be used as an ultraviolet shielding additive in outdoor PVC materials or special places.
Detailed Description
The invention will be further described with reference to specific examples, but is not limited thereto.
The materials according to the embodiments of the present invention are known and commonly available, and may be purchased conventionally, unless otherwise specified.
Example 1
0.9g of manganese acetate tetrahydrate and 0.15g of o-phenylenediamine are stirred in 45mL of ethanol to be completely dissolved. Adding into a polytetrafluoroethylene high-pressure reaction kettle, preserving heat at 180 ℃ for reaction for 12 hours, centrifuging, washing and drying to obtain Mn-CDs (marked as S1)
1.29g Mn-CDs were added to 50mL heptane and 16mL polyoxyethylene lauryl ether. Stirring and mixing uniformly at room temperature, dripping 2.5mL of ultrapure water and 0.5mL of concentrated ammonia water, stirring for 1h, adding 1.5mL of TEOS, keeping the reaction for 72h under stirring, adding about 30mL of ethanol to precipitate microemulsion, centrifuging, washing and drying to obtain Mn-CDs@SiO 2 (denoted as M1).
0.25g Mn-CDs@SiO 2 Dissolved in 20mL of 0.1mol/L CaCl 2 The solution was stirred and mixed well and 20mL of 0.1mol/LNa was added rapidly 2 CO 3 Reacting for 24h under 1000rpm magnetic stirring, centrifuging, washing and drying to obtain solid powder Mn-CDs@SiO 2 @CaCO 3 (denoted SL 1).
20mL 0.1mol/L CaCl 2 20mL of 0.1mol/LNa was added rapidly with stirring 2 CO 3 The solution is reacted for 24 hours under 1000rpm magnetic stirring, centrifuged, washed and dried to obtain pure CaCO 3 。
Example two
0.40g Mn-CDs@SiO 2 Dissolved in 20mL of 0.1mol/L CaCl 2 The solution was stirred and mixed well and 20mL of 0.1mol/LNa was added rapidly 2 CO 3 The medium solution reacts for 24 hours under 1000rpm magnetic stirring, and is centrifuged, washed and dried to obtain solid powder Mn-CDs@SiO 2 @CaCO 3 (denoted SL 2).
Example III
And (3) preparing the PVC composite film.
The weighed nano particles are respectively washed by a small amount of acetone in an ultrasonic manner and centrifuged for subsequent use.
0.8g of PVC powder is slowly added into 10mL of DMF under stirring, and the mixture is stirred and dispersed uniformly.
The specified amount of nano particles are dissolved in 10mL of DMF, the mixture is evenly dispersed by ultrasonic, and then added into the PVC solution, and after stirring for 2 hours, the mixture is further subjected to ultrasonic treatment for 0.5 hour to obtain a dispersion liquid.
And pouring the dispersion liquid on a culture dish, naturally cooling and shaping for 20min in air, changing water for many times for soaking, and drying for 24h at 50 ℃ in an oven to obtain the PVC/ultraviolet absorbent composite film (50+/-10 mu m) with uniform thickness.
The pure PVC film is prepared by the same method, and ultraviolet shielding performance test and comparison are carried out.
As can be seen from the test results of the above examples, mn-CDs and SiO 2 The ultraviolet shielding capability is obviously improved after combination, a remarkable synergistic effect is generated, and the effective shielding of PVC to ultraviolet rays can be realized by adjusting the content of the calcium carbonate compound and the thickness of the film.
Drawings
FIG. 1 is an infrared spectrum of S1, M1 and SL1 prepared in example one.
FIG. 2 is a schematic diagram of S1, M1, SL2 and pure CaCO prepared in example one and example two 3 Is light absorbing by solid ultravioletA spectrogram.
FIG. 3 is a graph of ultraviolet transmission spectra of the PVC film prepared in example three and a (2%) nanoparticle/PVC composite film.
FIG. 4 is a graph of ultraviolet transmission spectra of different SL2/PVC composite films prepared in example three.
Claims (9)
1. The preparation method of the calcium carbonate composite material with the ultraviolet shielding performance is characterized by comprising the following synthesis steps:
(1) Manganese acetate tetrahydrate (MnC) 4 H 6 O 4 ·4H 2 O) and O-phenylenediamine (C) 6 H 8 N 2 ) Dissolving in absolute ethyl alcohol, carrying out solvothermal reaction for 12 hours at 180 ℃, centrifuging, washing and drying to obtain the manganese-doped carbon quantum dots (Mn-CDs).
(2) Mn-CDs, heptane and polyoxyethylene lauryl ether are stirred and mixed uniformly, ultrapure water and concentrated ammonia water are dripped into the mixture, ethyl orthosilicate is added after stirring for 1h, the reaction is continued for 72h under stirring at room temperature, ethanol is added to lead the microemulsion to be completely precipitated, and Mn-CDs@SiO is obtained after centrifugation, washing and drying 2 。
(3)Mn-CDs@SiO 2 Dissolving in CaCl 2 Stirring and mixing the solution uniformly, and rapidly adding Na 2 CO 3 The solution is reacted for 24 hours at room temperature under 1000rpm magnetic stirring, and is centrifuged, washed and dried to obtain Mn-CDs@SiO 2 @CaCO 3 。
2. The calcium carbonate composite material with ultraviolet shielding performance and the preparation method thereof according to claim 1, wherein the experimental water is self-made ultrapure water.
3. The calcium carbonate composite material having ultraviolet shielding property and the preparation method thereof according to claim 1, wherein, preferably, in the step (1), the mass ratio of manganese acetate tetrahydrate and o-phenylenediamine=6g: 1g, molar volume ratio of manganese acetate tetrahydrate to absolute ethanol = 1mmol: (10-12) mL.
4. The calcium carbonate composite material with ultraviolet shielding property and the preparation method thereof according to claim 1, wherein, preferably, in the step (2), the mass-volume ratio of Mn-CDs, heptane, polyoxyethylene lauryl ether=1g: (35-40) mL: (10-15) mL, volume ratio of heptane and ultrapure water, concentrated ammonia water = 1mL:0.05mL:0.01ml, mass to volume ratio of mn-CD and ethyl orthosilicate = 1g: (1.0-1.2) mL.
5. The method of producing a calcium carbonate composite material having ultraviolet shielding properties according to claim 1, wherein, preferably, caCl in step (3) 2 And Na (Na) 2 CO 3 Volume ratio of solution = 1:1, the concentration of the two is 0.1mol/L, mn-CDs@SiO 2 And CaCl 2 Mass volume ratio of solution= (0.01-0.02) g:1mL.
6. The method of producing a calcium carbonate composite material having ultraviolet shielding properties according to claim 1, wherein the washing in each step is preferably performed by washing with water and then with absolute ethanol.
7. The calcium carbonate composite material having ultraviolet shielding property and the method for producing the same according to claim 1, wherein the drying temperature in steps (1), (2) and (3) is preferably 60 to 70 ℃.
8. The method for preparing the calcium carbonate composite material with ultraviolet shielding performance according to claim 1, wherein the method is simple in steps, strong in operability and CaCO 3 Free radicals are not generated when the base material is irradiated or heated, the base material has excellent corrosion resistance and heat resistance, and photo (thermal) catalytic degradation of the base material can be effectively avoided.
9. The method for preparing a calcium carbonate composite material with ultraviolet shielding performance according to claim 1, wherein the prepared CaCO is 3 The composite material has excellent ultraviolet shielding performance and is endowed with PVC in common useCaCO (R) as an additive 3 The novel performance is an innovative application of the inorganic quantum dots, expands CaCO 3 The ultraviolet shielding additive can be used as an ultraviolet shielding additive in PVC materials in outdoor or special places in the application range of the PVC and other material fields.
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| CN202310730378.6A CN116731392A (en) | 2023-06-20 | 2023-06-20 | Calcium carbonate composite material with ultraviolet shielding performance and preparation method thereof |
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| CN202310730378.6A CN116731392A (en) | 2023-06-20 | 2023-06-20 | Calcium carbonate composite material with ultraviolet shielding performance and preparation method thereof |
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