CN111286085A - Lipophilic polyacrylate coated calcium carbonate composite material and preparation and application thereof - Google Patents
Lipophilic polyacrylate coated calcium carbonate composite material and preparation and application thereof Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/10—Treatment with macromolecular organic compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
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Abstract
The invention relates to a lipophilic polyacrylate coated calcium carbonate composite material and preparation and application thereof, wherein 100 parts of calcium carbonate; 50-350 parts of polyacrylate solution; 0.5-3 parts of sodium dodecyl sulfate; 20-200 parts of sodium hydroxide solution. Uniformly dispersing calcium carbonate powder and sodium dodecyl sulfate in a deionized water solution, adding a polyacrylate solution, and performing ultrasonic dispersion; dropwise adding a sodium hydroxide solution at constant temperature and constant speed, carrying out suction filtration to collect white solids, washing the product to be neutral by using deionized water, carrying out ultrasonic dispersion, and drying by using a freeze dryer to obtain the product. The method has the characteristics of simple operation, environmental friendliness and outstanding pertinence, and the obtained product has good stability, strong applicability, good dispersibility and better application prospect.
Description
Technical Field
The invention belongs to the field of modified calcium carbonate composite materials and preparation and application thereof, and particularly relates to a lipophilic polyacrylate coated calcium carbonate composite material and preparation and application thereof.
Background
Calcium carbonate as an inorganic compound has the characteristics of low price, no toxicity, no odor, high whiteness, good hardness and the like, and is widely applied to the production process of rubber and plastics. It is statistically estimated that calcium carbonate accounts for about 70% of the amount of inorganic filler used in the manufacturing process of plastic articles. Meanwhile, the surface of calcium carbonate has hydrophilic and oleophobic properties, the affinity with polar organic polymers is poor, and the dispersion is uneven or accumulation phenomenon is easily caused in a base material, so that a dissimilar interface is generated between a filler and the polymers, and the defect easily generates stress concentration, so that the mechanical property of the filled composite material is reduced, and the fracture phenomenon is generated. Generally, various modifying agents are added to modify the surface of calcium carbonate, and patent application No. 201810644633.4 discloses a preparation method of graphene grafted modified calcium carbonate, wherein a silane coupling agent is coated on the surface of calcium carbonate to enable the calcium carbonate to have the condition of grafting with graphene, calcined argil, carbon nanotubes and plant ash are added to improve the compatibility of calcium carbonate and a rubber matrix, and the prepared composite material has good hardness, wear resistance and reinforcing performance; other commonly used modifiers are surfactants, coupling agents, etc., of which resin acids (salts) and fatty acids (salts) are most widely used. Application No. 201710915914.4 discloses a method for preparing modified light calcium carbonate, wherein sodium oleate is used as modifier to organize the surface of calcium carbonate, so that the surface of calcium carbonate particles has certain hydrophilic and oleophobic properties, and simultaneously, the modified light calcium carbonate is mixed with triethyl citrate, styrene, organic bentonite and other substances, thereby solving the problems of poor hydrophilic and oleophobic properties, poor dispersibility, easy sedimentation and the like of light calcium carbonate, and improving the application range of the light calcium carbonate; however, the currently used modifier generally has a short organic chain, a good interface layer cannot be formed between the surface of the treated calcium carbonate and the resin, the effective concentration of the interface is obviously reduced under the condition that the amount of the calcium carbonate in the system is added, and a uniform and effective elastomer cannot be formed on the surface of the calcium carbonate, so that the function of an organic product is influenced.
Disclosure of Invention
The invention aims to solve the technical problem of providing an oleophilic polyacrylate coated calcium carbonate composite material and preparation and application thereof, and overcomes the defects that a modifier in the prior art is generally short in organic chain and a good interface layer cannot be formed between the treated calcium carbonate surface and resin.
The invention discloses a calcium carbonate composite material which is characterized by comprising the following raw materials in parts by weight:
preferably, the raw material components comprise, by weight:
the calcium carbonate is 500-800 mesh calcium carbonate.
The polyacrylate solution had a solids content of 34%.
The mass percentage concentration of the sodium hydroxide solution is 20%.
The preparation method of the calcium carbonate composite material comprises the following steps:
(1) uniformly dispersing calcium carbonate and sodium dodecyl sulfate in a deionized water solution, magnetically stirring, adding a polyacrylate solution, magnetically stirring, and ultrasonically dispersing;
(2) and (2) dropwise adding a sodium hydroxide solution into the solution obtained in the step (1) at a constant speed, stirring at a constant temperature, filtering, collecting filtrate, fully washing the filtrate with deionized water to be neutral, dispersing the filtrate in the deionized water, uniformly dispersing the filtrate by ultrasonic waves, pre-freezing at a low temperature, and drying to obtain the calcium carbonate composite material.
The preferred mode of the above preparation method is as follows:
the solid content of the polyacrylate solution in the step (1) is 34%.
The magnetic stirring time in the step (1) is 5-10 min.
And (2) ultrasonically dispersing for 15-20min in the step (1).
And (3) finishing the dropwise addition of the sodium hydroxide solution in the step (2) for 1-5 minutes.
The constant-temperature stirring temperature in the step (2) is 20-25 ℃; the ultrasonic uniform dispersion time is 30-40 min; the low-temperature pre-freezing temperature is below-75 ℃; the drying is freeze dryer drying.
The invention provides an application of the calcium carbonate composite material.
The specific preparation method of the polyacrylate used in the invention comprises the following steps: uniformly mixing n-butyl acrylate, styrene, methyl methacrylate, acrylic acid, a part of emulsifier, diacetone acrylamide and deionized water, and pre-emulsifying to obtain pre-emulsion; wherein part of the emulsifier accounts for 1-7% of the total mass of the monomers; stirring sodium bicarbonate, deionized water and the rest of emulsifier at constant temperature, adding part of pre-emulsion and initiator aqueous solution, stirring at constant temperature, dropwise adding the rest of pre-emulsion and initiator aqueous solution, keeping the temperature, cooling, adjusting pH, adding polyorganosiloxane, stirring for dissolving, stopping heating, and filtering to obtain the final product.
Advantageous effects
(1) The invention adopts the method of coating calcium carbonate with polyacrylate solution to prepare the polyacrylate coated calcium carbonate composite material, solves the problems that the calcium carbonate is hydrophilic and a good interface layer cannot be formed between the calcium carbonate and an organic polymer material, and the like, and the modification method is not reported in related patents, has the advantages of simple and convenient operation, low cost, easy popularization, no toxicity, environmental protection and excellent stability, and improves the application range of the calcium carbonate.
(2) Compared with the unmodified calcium carbonate material, the polyacrylate-coated calcium carbonate composite material prepared by the invention has the following excellent characteristics:
① the infrared spectrum of the composite material shows that the calcium carbonate has a peak at 1733cm-1The ester group-C ═ O stretching vibration absorption peak appears at 1166cm-1C-O-C telescopic vibration absorption peaks appear at the positions, which shows that the polyacrylate is successfully coated on the zinc stearate;
② the contact angle of the prepared composite material can reach 102.1 degrees, which shows that the composite material has certain lipophilicity, and the contact angle of calcium carbonate is 50.4 degrees.
③ after the surface appearance of the composite material is enlarged by 100000 times, a large amount of wool-like attachments are observed on the surface of the material under SEM, which shows that the polyacrylate is coated on the surface of calcium carbonate more uniformly.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is the contact angle of the product of example 3; a: calcium carbonate contact angle (50.4 °); b: example 3 product contact angle (102.1 °);
FIG. 3 is an infrared spectrum of the product of example 3;
fig. 4 is an SEM picture of the product of example 3.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The invention adopts 800-mesh light calcium carbonate produced by Henan chemical industry; other monomers and additives such as emulsifier come from the national medicine group and are chemically pure.
The specific preparation method of the polyacrylate comprises the following steps: 10g of n-butyl acrylate, 4.8g of styrene, 7.3g of methyl methacrylate, 0.7g of acrylic acid, 0.4g of sodium dodecyl sulfate, 0.06g of polyoxyethylene octylphenol ether-10 and 11g of deionized water are uniformly mixed in a beaker, and the mixture is magnetically stirred for 20min for pre-emulsification. Respectively dissolving 0.072g of potassium persulfate in 2g of deionized water, and dissolving 0.09g of potassium persulfate in 5.4g of deionized water for later use; uniformly mixing 0.09g of sodium bicarbonate, 9.6g of deionized water, 0.046g of sodium dodecyl sulfate and 0.07g of polyoxyethylene octyl phenol ether-10 in a four-neck flask, controlling the temperature to be 82 ℃, and stirring for 15min at constant temperature, wherein the rotating speed is 350 rpm; when the emulsifier is completely dissolved, adding 2.8g of pre-emulsion and 2.2g of potassium persulfate aqueous solution at one time, and stirring for 30min at constant temperature; respectively and simultaneously dripping the residual emulsion and 5.5g of potassium persulfate solution into a four-neck flask, finishing dripping within 3 hours, then preserving the temperature for 1.5 hours, cooling to 55 ℃, and adjusting the pH value to 8-9 by using ammonia water; adding 1.4g of polyorganosiloxane, fully stirring for 30min, stopping heating, filtering, and discharging.
Example 1
(1) Uniformly mixing 5g of commercially available calcium carbonate, 0.05g of sodium dodecyl sulfate and 45g of deionized water in a beaker, magnetically stirring for 10min, adding 2.5g of polyacrylate solution, magnetically stirring for 10min, and ultrasonically dispersing for 20 min;
(2) 6g of sodium hydroxide solution with the mass fraction of 20 percent is added into the mixed solution, and the mixture is magnetically stirred for 15min at the temperature of 20 ℃.
(3) The mixture was filtered, the white filtrate was collected and washed thoroughly with deionized water.
(4) Collecting the product, dispersing in 15g of deionized water, and performing ultrasonic dispersion for 30 min; pre-freezing at-75 deg.C, drying with freeze dryer, and collecting product.
FIG. 1 is a process flow diagram of the present invention.
Example 2
(1) Uniformly mixing 5g of commercially available calcium carbonate, 0.05g of sodium dodecyl sulfate and 45g of deionized water in a beaker, magnetically stirring for 10min, adding 5.0g of polyacrylate solution, magnetically stirring for 10min, and ultrasonically dispersing for 20 min;
(2) 6g of sodium hydroxide solution with the mass fraction of 20 percent is added into the mixed solution, and the mixture is magnetically stirred for 15min at the temperature of 20 ℃.
(3) The mixture was filtered, the white filtrate was collected and washed thoroughly with deionized water.
(4) Collecting the product, dispersing in 15g of deionized water, and performing ultrasonic dispersion for 30 min; pre-freezing at-75 deg.C, drying with freeze dryer, and collecting product.
Example 3
(1) Uniformly mixing 5g of commercially available calcium carbonate, 0.05g of sodium dodecyl sulfate and 45g of deionized water in a beaker, magnetically stirring for 10min, adding 7.5g of polyacrylate solution, magnetically stirring for 10min, and ultrasonically dispersing for 20 min;
(2) 6g of sodium hydroxide solution with the mass fraction of 20 percent is added into the mixed solution, and the mixture is magnetically stirred for 15min at the temperature of 20 ℃.
(3) The mixture was filtered, the white filtrate was collected and washed thoroughly with deionized water.
(4) Collecting the product, dispersing in 15g of deionized water, and performing ultrasonic dispersion for 30 min; pre-freezing at-75 deg.C, drying with freeze dryer, and collecting product.
As shown in fig. 2, the product has a certain lipophilicity; FIGS. 3 and 4 show that the polyacrylate has been coated relatively uniformly on the surface of the calcium carbonate.
Comparative example 1
(1) Uniformly mixing 5g of commercially available calcium carbonate, 0.05g of sodium dodecyl sulfate and 45g of deionized water in a beaker, magnetically stirring for 10min, adding 7.5g of deionized water again, magnetically stirring for 10min, and ultrasonically dispersing for 20 min;
(2) 6g of sodium hydroxide solution with the mass fraction of 20 percent is added into the mixed solution, and the mixture is magnetically stirred for 15min at the temperature of 20 ℃.
(3) The mixture was filtered, the white filtrate was collected and washed thoroughly with deionized water.
(4) Collecting the product, dispersing in 15g of deionized water, and performing ultrasonic dispersion for 30 min; pre-freezing at-75 deg.C, drying with freeze dryer, and collecting product.
Table 1 shows the dispersibility of the composite materials prepared in the embodiments 1 to 3 and the comparative example 1 in deionized water. The activation index test was carried out in accordance with the relevant provisions of "industrially active precipitated calcium carbonate" in HG/T2567-94. Accurately weighing 3.0g of sample, placing the sample in a 250ml separating funnel, adding 200ml of deionized water, fully shaking up, placing the sample on a funnel stand for standing for 15min, placing the precipitated calcium carbonate at the lower layer into a crucible which is completely dried, placing the crucible in a 105 ℃ blast drying oven, drying to constant weight, and weighing.
In the formula: h-activation rate of powder,%;
M2-drying the crucible and-modifying the mica powder mass, g;
M1-crucible mass, g;
m represents the mass of the sample, g.
Table 1:
| example 1 | Example 2 | Example 3 | Comparative example 1 | |
| Amount of acrylate emulsion added (%) | 50％ | 100％ | 150％ | 0％ |
| Activation index (%) | 32.4 | 57.1 | 69.2 | 64.9 |
| Contact angle (°) | 69.9 | 84.2 | 102.1 | 50.4 |
As can be seen from the table, the product obtained by the present invention has better lipophilicity and dispersibility in organic solvents than the comparative example.
Claims (10)
1. The calcium carbonate composite material is characterized by comprising the following raw material components in parts by weight:
2. the composite material of claim 1, wherein the raw material components comprise, in parts by weight:
3. the composite material of claim 1, wherein the raw material components comprise, in parts by weight:
4. the composite material of claim 1, wherein the calcium carbonate is 500-800 mesh calcium carbonate.
5. A method for preparing the calcium carbonate composite material of claim 1, comprising:
(1) uniformly dispersing calcium carbonate and sodium dodecyl sulfate in a deionized water solution, magnetically stirring, adding a polyacrylate solution, magnetically stirring, and ultrasonically dispersing;
(2) and (2) dropwise adding a sodium hydroxide solution into the solution obtained in the step (1) at a constant speed, stirring at a constant temperature, filtering, collecting filtrate, fully washing the filtrate with deionized water to be neutral, dispersing the filtrate in the deionized water, uniformly dispersing the filtrate by ultrasonic waves, pre-freezing at a low temperature, and drying to obtain the calcium carbonate composite material.
6. The method according to claim 5, wherein the polyacrylate solution in the step (1) has a solid content of 34%.
7. The method according to claim 5, wherein the ultrasonic dispersion in the step (1) is carried out for 15-20 min.
8. The method according to claim 5, wherein the sodium hydroxide solution in the step (2) has a solid content of 20% and is added dropwise over 1 to 5 minutes.
9. The preparation method according to claim 5, wherein the constant-temperature stirring temperature in the step (2) is 20-25 ℃; the ultrasonic uniform dispersion time is 30-40 min; the low-temperature pre-freezing temperature is below-75 ℃; the drying is freeze dryer drying.
10. Use of the calcium carbonate composite material according to claim 1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113522931A (en) * | 2021-07-09 | 2021-10-22 | 浙江工业大学 | Mineral oxidation acid production inhibition method based on in-situ rapid film formation on surface of sulfurized mineral |
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| CN1482172A (en) * | 2003-07-22 | 2004-03-17 | 四川大学 | polyacrylic ester/inorganics I/inorganics II ternary compound particle and process for producing the same |
| CN102464786A (en) * | 2010-11-10 | 2012-05-23 | 上海华明高技术（集团）有限公司 | Polyacrylate elastomer emulsion and preparation method thereof |
| WO2019197520A1 (en) * | 2018-04-11 | 2019-10-17 | Omya International Ag | Calcium carbonate comprising composition for elastomeric film preparation |
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2020
- 2020-02-28 CN CN202010127159.5A patent/CN111286085A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1482172A (en) * | 2003-07-22 | 2004-03-17 | 四川大学 | polyacrylic ester/inorganics I/inorganics II ternary compound particle and process for producing the same |
| CN102464786A (en) * | 2010-11-10 | 2012-05-23 | 上海华明高技术（集团）有限公司 | Polyacrylate elastomer emulsion and preparation method thereof |
| WO2019197520A1 (en) * | 2018-04-11 | 2019-10-17 | Omya International Ag | Calcium carbonate comprising composition for elastomeric film preparation |
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| 沈春林 主编: "《防水密封材料手册》", 30 June 2000, 中国建材工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113522931A (en) * | 2021-07-09 | 2021-10-22 | 浙江工业大学 | Mineral oxidation acid production inhibition method based on in-situ rapid film formation on surface of sulfurized mineral |
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