CN-122011749-A - Nylon material containing modified calcium carbonate

Abstract

The application belongs to the technical field of preparation of high polymer materials, and particularly relates to a nylon material containing modified calcium carbonate. The nylon material is prepared by adding calcium carbonate into absolute ethyl alcohol, adding stearic acid for reaction to obtain pretreated calcium carbonate, adding pretreated calcium carbonate into an ethanol-water mixed solution, adding boric acid and urea, carrying out ultrasonic dispersion and hydrothermal reaction to obtain a calcium carbonate load boron-nitrogen compound, dissolving polyether block polyamide in DMSO, adding furancarboxylic acid for reaction for 20-24 hours, adding calcium carbonate load boron-nitrogen compound, stirring for 2-3 hours, drying to obtain modified calcium carbonate, melt-blending nylon and maleimide end-capped compound to obtain modified nylon, dry-blending the modified nylon obtained in the step S4, an antioxidant and a lubricant, then melt-blending the modified calcium carbonate, extruding and granulating to obtain the nylon material containing the modified calcium carbonate. The nylon material containing the modified calcium carbonate has the effects of rigidity and toughness balance and high heat conduction.

Inventors

• LI YONGQUAN
• LI QING
• LI XIANGKE

Assignees

• 临沂富阳碳酸钙有限公司

Dates

Publication Date

20260512

Application Date

20260320

Claims (10)

1. 1. The nylon material containing the modified calcium carbonate is characterized by being prepared by the following steps: s1, adding calcium carbonate into absolute ethyl alcohol for ultrasonic dispersion, adding stearic acid for reaction, carrying out suction filtration, washing and drying to obtain pretreated calcium carbonate; S2, dispersing the pretreated calcium carbonate in an ethanol-water mixed solution, adding boric acid and urea, performing hydrothermal reaction after ultrasonic dispersion, centrifuging, washing and drying to obtain a calcium carbonate-loaded boron-nitrogen compound; S3, dissolving polyether block polyamide in DMSO, adding furanic acid, heating to 80-85 ℃, adding EDC and NHS to catalyze amidation reaction for 20-24h, then adding calcium carbonate to load boron-nitrogen compound, stirring for 2-3h, and spray drying to obtain modified calcium carbonate; S4, adding 90-100 parts of nylon and 3-5 parts of maleimide end-capping compound into a double-screw extruder according to parts by weight, and carrying out melt blending to obtain modified nylon; s5, dry-mixing the modified nylon obtained in the step S4, 1-2 parts of antioxidant and 1-2 parts of lubricant according to parts by mass, adding into a double-screw extruder, adding 5-6 parts of modified calcium carbonate, melt-blending, extruding and granulating to obtain the nylon material containing the modified calcium carbonate.
2. 2. A modified calcium carbonate containing nylon material according to claim 1, wherein the mass ratio of stearic acid to calcium carbonate is 100:1-2.
3. 3. The modified calcium carbonate containing nylon material according to claim 1, wherein the mass ratio of the pretreated calcium carbonate, boric acid and urea is 100:10-15:30-45.
4. 4. A modified calcium carbonate containing nylon material according to claim 1, wherein the polyether block polyamide has a molar ratio to furancarboxylic acid of from 1:1.1 to 1.2.
5. 5. The modified calcium carbonate containing nylon material of claim 1, wherein the molar ratio of EDC, NHS, furancarboxylic acid is 1-1.2:1-1.2:1.
6. 6. The modified calcium carbonate-containing nylon material according to claim 1, wherein the mass ratio of the calcium carbonate-supported boron nitrogen compound to the polyether block polyamide is 0.8-1:1.
7. 7. A modified calcium carbonate containing nylon material according to claim 1, wherein the maleimide terminated polymer is a maleimide terminated poly (N-isopropylacrylamide) or a maleimide terminated caprolactam oligomer.
8. 8. The nylon material containing modified calcium carbonate according to claim 1, wherein the twin screw extruder of steps S4 and S5 has a feeding zone temperature of 220-230 ℃, a compression zone temperature of 240-250 ℃, a homogenizing zone temperature of 250-260 ℃, a die head temperature of 255-265 ℃ and a screw speed of 300-500 rpm.
9. 9. The modified calcium carbonate-containing nylon material according to claim 1, wherein the ultrasonic dispersion in step S2 is performed at a power of 200 to 400W for 15 to 20min.
10. 10. The modified calcium carbonate containing nylon material according to claim 1, wherein the hydrothermal reaction is carried out at a temperature of 180-185 ℃ for a time of 10-12 hours.

Description

Nylon material containing modified calcium carbonate Technical Field The application belongs to the technical field of preparation of high polymer materials, and particularly relates to a nylon material containing modified calcium carbonate. Background Nylon is one of five engineering plastics, and is widely applied to the fields of automobiles, electronics, aerospace and the like by virtue of the advantages of high strength, wear resistance, chemical corrosion resistance, easiness in processing and the like. However, pure nylon has the defects of strong hygroscopicity, insufficient heat resistance, high notch sensitivity and the like, and is difficult to meet the requirements of high-end scenes on light weight, multiple functions and long service life. The introduction of inorganic filler through filling modification is an important way for improving the performance of nylon, such as calcium carbonate, but the traditional technology faces the core challenges that the existing modification method adopts a coupling agent or polymer coating to improve the dispersibility, but the interface bonding is still mainly physical adsorption or hydrogen bonding and is easy to dissociate under the stress or high temperature, so that the tensile strength of the composite material is limited, the toughness is obviously reduced, the function is single, the rigidity-toughness is difficult to cooperate, and the rigidity-toughness balance is difficult. In view of the above challenges, development of a multifunctional integrated nylon composite material with strong interface bonding, rigidity and toughness balance, green process and the like is needed. Disclosure of Invention The application aims to provide a nylon material containing modified calcium carbonate, which has the effects of rigidity and toughness balance and high heat conduction. In order to achieve the above object, the present application provides a nylon material containing modified calcium carbonate, which is prepared by the following steps: s1, adding calcium carbonate into absolute ethyl alcohol for ultrasonic dispersion, adding stearic acid for reaction, carrying out suction filtration, washing and drying to obtain pretreated calcium carbonate; In the process, the stearic acid carboxyl and calcium ions form hydrophobic calcium stearate which is stably attached to the surface of calcium carbonate. S2, dispersing the pretreated calcium carbonate in an ethanol-water mixed solution, adding boric acid and urea, performing hydrothermal reaction after ultrasonic dispersion, centrifuging, washing and drying to obtain a calcium carbonate-loaded boron-nitrogen compound; In the process, stearic acid isolates water molecules from the surface of calcium carbonate through a hydrophobic membrane, reduces hygroscopicity, is dispersed in a nonpolar medium through hydrophobic interaction, boric acid and urea react under hydrothermal conditions, urea is decomposed to generate ammonia gas and isocyanic acid, the ammonia gas and the isocyanic acid are further condensed with boric acid to generate a precursor, and finally, the precursor is dehydrated to form a calcium carbonate-loaded boron-nitrogen compound, and unreacted boric acid/urea remains on the surface of the boron-nitrogen compound in the synthesis process to form polar functional groups such as hydroxyl groups, amino groups, boron-oxygen bonds and the like which can form intermolecular hydrogen bonds with residual hydroxyl groups on the surface of the calcium carbonate, so that the polar functional groups are anchored on the surface of the calcium carbonate. S3, dissolving polyether block polyamide in DMSO, adding furanic acid, heating to 80-85 ℃, adding EDC and NHS to catalyze amidation reaction for 20-24h, then adding calcium carbonate to load boron-nitrogen compound, stirring for 2-3h, and spray drying to obtain modified calcium carbonate; In the process, the polyether block polyamide contains amino and carboxyl of furancarboxylic acid to undergo condensation reaction under the catalysis of EDC and NHS, EDC activates the carboxyl of furancarboxylic acid to form an unstable O-acyl isourea intermediate, NHS is substituted to generate stable N-hydroxysuccinimide ester, the stable N-hydroxysuccinimide ester reacts with the amino of the polyether block polyamide to form an amide bond, a polyether block polyamide-furancarboxylic acid compound is formed, hydrogen bond bonding is formed between the polyether block polyamide-furancarboxylic acid compound and polar groups on the surface of a calcium carbonate-loaded boron-nitrogen compound, and a coating layer is formed after spray drying. S4, adding 90-100 parts of nylon and 3-5 parts of maleimide end-capping compound into a double-screw extruder according to parts by weight, and carrying out melt blending to obtain modified nylon; In the process, nylon and maleimide end-capping compound are melt blended, and the terminal amino group of the nylon and maleimide group are sub