CN110591247A - Multi-scale composite thermal-reversible cross-linked porcelainized PVC material - Google Patents
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Abstract
The invention relates to a multi-scale composite thermal reversible crosslinking porcelainized PVC material. The raw materials comprise PVC, wollastonite, montmorillonite, talcum powder, a porcelain-forming auxiliary agent, a heat reversible cross-linking agent and other auxiliary agents; the particle sizes of the montmorillonite, the talcum powder, the wollastonite and the ceramic forming auxiliary agent have gradient difference. The nano montmorillonite has good enhancing and sintering-assisting functions; wollastonite plays a good role in supporting a framework in the PVC sintering process; the superfine talcum powder can reduce the torque and friction borne by the screw rod when the materials are melted and blended in the double-screw extruder, improve the mixing efficiency and simultaneously reduce the requirement on double-screw equipment and the abrasion on the equipment; the gradient change of the particle sizes among different fillers can enable the fillers with small particle sizes to be filled in gaps formed by the fillers with large particle sizes, and the 'gap filling' effect formed among the fillers can effectively reduce the melt index of a filled PVC melt, so that the extrusion process of porcelainized PVC is easier to control, the surface of a material is smoother, and the defects are few.
Description
Technical Field
The invention relates to the technical field of functional polymer composite materials, in particular to a preparation method of a multi-scale composite thermal reversible crosslinked porcelainized PVC material.
Background
Polyvinyl chloride (PVC) is one of five common plastics, and the demand is second to polyethylene. In China, PVC is still the resin with the largest yield at present. Polyvinyl chloride (PVC) resin is a polar non-crystalline polymer, and the product has good physical properties and chemical properties, can be widely applied to the fields of industry, construction, agriculture, daily necessities and the like, wherein about 7 percent of the total amount of PVC is used for wire and cable materials.
Along with the continuous development of economy in China, the process of urbanization is continuously promoted, and the trend of urban population densification is increased. The residential buildings and public buildings are also developed towards high-rise, intensive and function-diversified directions. A large amount of building materials, especially finishing materials, are widely used, and the possibility of causing fire is increasing. About 12 thousands of fires occur in the country every year, about 200 million yuan is lost every year, and about 2500 casualties occur. At present, the market demand of the fireproof cable is 200 plus 300 million RMB every year, and the fireproof cable is mainly used in special fields with higher requirements on fireproof safety, such as subway traffic, tunnels, large-scale power plants and the like. Along with the improvement of the fire-proof safety consciousness, the requirements on the aspects of large-scale public place buildings, civil buildings and the like are more and more, so that the market demand is further expanded, and the porcelainized PVC fire-proof insulating material has great cost and comprehensive performance advantages in the aspect of popularization and promotion of fire-proof cables. However, the PVC itself has a low heat-resistant temperature, which affects the temperature application range. In order to increase the application temperature, a crosslinking method is generally adopted. At present, the most adopted crosslinking mode is chemical crosslinking or irradiation crosslinking, however, another problem is brought after crosslinking, namely PVC cannot be recycled after crosslinking, and the sustainable, green and circular economy development trend advocated at present is not met.
Therefore, the thermally reversible crosslinked porcelainized fireproof PVC material can not only improve the use temperature of the porcelainized PVC material, but also keep the recycling performance of PVC, and has important market value in the field of low-cost fireproof polymers.
Disclosure of Invention
The invention aims at the current market and policy guidance and provides a preparation method of a multi-scale composite filling thermal reversible crosslinking porcelainized PVC material.
The invention is realized by the following technical scheme: a multi-scale composite thermal reversible crosslinking porcelainized PVC material comprises raw materials of PVC, wollastonite, montmorillonite, talcum powder, a porcelainizing auxiliary agent, a thermal reversible crosslinking agent and other auxiliary agents;
the particle sizes of the montmorillonite, the talcum powder, the wollastonite and the ceramic forming auxiliary agent have gradient difference.
Furthermore, the montmorillonite is 80-400 nanometers, the talcum powder is 1-5 micrometers, the wollastonite is 5-10 micrometers, and the porcelain forming auxiliary agent is 10-40 micrometers.
Further, other auxiliaries include plasticizers and stabilizers;
the raw materials are proportioned according to the following mode in parts by weight:
100 portions of PVC
50-80 parts of wollastonite
5-15 parts of montmorillonite
3-10 parts of talcum powder
5-15 parts of porcelain forming auxiliary agent
10-25 parts of plasticizer
0.3-5 parts of stabilizer
1-5 parts of a thermal reversible cross-linking agent.
Furthermore, the montmorillonite is 80-400 nanometers, the talcum powder is 1-5 micrometers, the wollastonite is 5-10 micrometers, and the porcelain forming auxiliary agent is 10-40 micrometers.
Further, the polyvinyl chloride resin is a PVC resin with a polymerization degree of 500-2000.
Further, the wollastonite is a wollastonite long fiber, the diameter of the long fiber is 5-10 microns, the length-diameter ratio is 5 ~ 10, and the surface of the long fiber is modified by one or two of a silane coupling agent KH570, KH550 and a titanate coupling agent KR-138S, KR-TTS.
Furthermore, the montmorillonite is organic intercalation modified nano montmorillonite, the organic modifier is one of Dodecyl Trimethyl Ammonium Bromide (DTAB), hexadecyl trimethyl ammonium bromide (CTAB), Octadecyl Trimethyl Ammonium Bromide (OTAB) and octadecyl dimethyl benzyl ammonium chloride (ODBA), and the particle size of the modified montmorillonite is 80 ~ 400 nanometers.
Furthermore, the talcum powder is superfine talcum powder with the particle size of 1-5 microns, and the surface of the talcum powder is subjected to surface modification by one or two of silane coupling agent KH570, KH550 and titanate coupling agent KR-138S, KR-TTS.
Further, the ceramic forming auxiliary agent is composed of two or three of low-melting-point lead-free glass powder with a melting point of 400 ~ 800, zinc borate and chopped glass fiber powder, and the particle size range is 10-40 microns.
Further, the calcium zinc stabilizer is a solid composite calcium-zinc soap stabilizer, and comprises any of zinc stearate, calcium stearate, zinc laurate and calcium metasilicate.
Further, the thermal reversible cross-linking agent is long-chain binary tertiary amine, and the length of the fatty chain is 5-15 carbon atoms.
The invention relates to a preparation method of a multi-scale composite filling thermal reversible crosslinking porcelainized PVC fireproof material, which comprises the following steps:
1) adding the raw materials into a high-speed mixer, mixing for 15min at high speed, and discharging.
2) And adding the mixed materials into a double-screw extruder for melt blending, extruding and granulating after blending to obtain the multi-scale composite filling heat reversible crosslinking porcelainized PVC fireproof material granules, and further processing the granules into fire-resistant cables or test sample strips for testing various performances of the fire-resistant cables or test sample strips.
The invention has the beneficial effects that 1) the filler system used in the invention is skillfully designed, wherein: the nano montmorillonite has good enhancing and sintering-assisting functions; wollastonite with the length-diameter ratio of 5 to 10 can play a good skeleton supporting role in the PVC sintering process; the superfine talcum powder can reduce the torque and friction borne by the screw rod when the materials are melted and blended in the double-screw extruder, improve the mixing efficiency and simultaneously reduce the requirement on double-screw equipment and the abrasion on the equipment; the gradient change of the particle sizes among different fillers can enable the fillers with small particle sizes to be filled in gaps formed by the fillers with large particle sizes, and the 'gap filling' effect formed among the fillers can effectively reduce the melt index of a filled PVC melt, so that the extrusion process of porcelainized PVC is easier to control, the surface of a material is smoother, and the defects are few.
2) The invention replaces the traditional crosslinking by the thermal reversible crosslinking reaction, not only can improve the mechanical strength and the thermal stability of the porcelainized PVC material, but also can keep the recoverable characteristic of the PVC material, and is more environment-friendly.
3) The used filler or the auxiliary agent does not contain heavy metal lead, and is nontoxic and environment-friendly.
Detailed Description
Example 1:
a multi-scale composite filling thermal-reversible cross-linking porcelainized PVC fireproof material is prepared from the following raw materials in parts by weight: 100 parts of PVC with the polymerization degree of about 2000, 50 parts of wollastonite (the median particle size is 10 micrometers) with the surface treated by a silane coupling agent KH570 and a titanate coupling agent KR-138S, 15 parts of Dodecyl Trimethyl Ammonium Bromide (DTAB) intercalated modified montmorillonite (the median particle size is 400 nanometers), 3 parts of superfine talcum powder (the median particle size is 5 micrometers), 5 parts of a porcelain forming auxiliary agent (the weight ratio of low-melting-point lead-free glass to zinc borate to chopped glass fiber powder is 1:1: 1), 5 parts (the weight ratio of the median particle size is 40 micrometers), 35 parts of a plasticizer DOP, 5 parts of a stabilizer (the weight ratio of zinc stearate to calcium stearate is 2: 1), and 1 part of a thermal reversible crosslinking agent.
(1) Adding the raw materials into a high-speed mixer, mixing for 15min at high speed, and discharging.
(2) And adding the mixed materials into a double-screw extruder for melt blending, extruding and granulating after blending to obtain multi-scale composite filling heat reversible crosslinking porcelainized PVC fireproof material granules, further processing into test sample strips, and testing various performances of the test sample strips.
Example 2:
a multi-scale composite filling thermal-reversible cross-linking porcelainized PVC fireproof material is prepared from the following raw materials in parts by weight: 100 parts of PVC with the polymerization degree of about 500, 80 parts of wollastonite (with the median particle size of 5 micrometers) with the surface treated by a silane coupling agent KH550 and a titanate coupling agent KR-TTS, 5 parts of Octadecyl Trimethyl Ammonium Bromide (OTAB) intercalated modified montmorillonite (with the median particle size of 80 nanometers), 10 parts of superfine talcum powder (with the median particle size of 1 micrometer), 15 parts of a porcelain forming auxiliary agent (the weight ratio of low-melting-point lead-free glass to chopped glass fiber powder is 3: 1), 15 parts (with the median particle size of 10 micrometers), 25 parts of a plasticizer DOP, 0.3 part of a stabilizer (zinc laurate and calcium silicate in the weight ratio of 2: 1) and 5 parts of a thermal reversible crosslinking agent.
(1) Adding the raw materials into a high-speed mixer, mixing for 15min at high speed, and discharging.
(2) And adding the mixed materials into a double-screw extruder for melt blending, extruding and granulating after blending to obtain multi-scale composite filling heat reversible crosslinking porcelainized PVC fireproof material granules, further processing into test sample strips, and testing various performances of the test sample strips.
Example 3:
a multi-scale composite filling thermal-reversible cross-linking porcelainized PVC fireproof material is prepared from the following raw materials in parts by weight: 100 parts of PVC with the polymerization degree of about 1000, 60 parts of wollastonite (with the median particle size of 8 micrometers) with the surface treated by a titanate coupling agent KR-TTS, 10 parts of hexadecyl trimethyl ammonium bromide (CTAB) intercalated modified montmorillonite (with the median particle size of 200 nanometers), 8 parts of superfine talcum powder (with the median particle size of 3 micrometers), 10 parts of a porcelain forming auxiliary agent (low-melting-point lead-free glass: zinc borate with the weight ratio of 2: 1) (with the median particle size of 25 micrometers), 20 parts of a plasticizer DOP, 3 parts of a stabilizer (zinc stearate, calcium metasilicate with the weight ratio of 2: 1) and 3 parts of a thermally reversible crosslinking agent.
(1) Adding the raw materials into a high-speed mixer, mixing for 15min at high speed, and discharging.
(2) And adding the mixed materials into a double-screw extruder for melt blending, extruding and granulating after blending to obtain multi-scale composite filling heat reversible crosslinking porcelainized PVC fireproof material granules, further processing into test sample strips, and testing various performances of the test sample strips.
While the invention has been described with reference to specific embodiments thereof, it will be understood by those skilled in the art that various changes and modifications may be made therein without departing from the spirit of the invention, and it is intended to cover all such modifications and alterations as fall within the true scope of the invention.
The test results of the sample band performance obtained in the above example are as follows:
| tensile strength MPa | Elongation% | Vicat heat resistance (DEG C) | Hardness of sintering | Whether or not to be recycled | Surface of | |
| Example 1 | 12.4 | 275 | 87.5 | Hard | Is that | Smooth and flawless |
| Example 2 | 8.7 | 214 | 73.7 | Hard | Is that | Smooth and flawless |
| Example 3 | 11.2 | 237 | 82.8 | Hard | Is that | Smooth and flawless |
Claims (10)
1. A multi-scale composite thermal reversible crosslinking porcelainized PVC material is characterized in that the raw materials comprise PVC, wollastonite, montmorillonite, talcum powder, a porcelainizing auxiliary agent, a thermal reversible crosslinking agent and other auxiliary agents;
the particle sizes of the montmorillonite, the talcum powder, the wollastonite and the ceramic forming auxiliary agent have gradient difference.
2. The multi-scale composite thermal reversible crosslinked porcelainized PVC material according to claim 1, wherein the montmorillonite is 80-400 nm, the talcum powder is 1-5 microns, the wollastonite is 5-10 microns, and the porcelain forming aid is 10-40 microns.
3. The multi-scale composite thermoreversibly cross-linked ceramifiable PVC material as claimed in claim 1, wherein the other auxiliary agents include plasticizers and stabilizers;
the raw materials are proportioned according to the following mode in parts by weight:
100 portions of PVC
50-80 parts of wollastonite
5-15 parts of montmorillonite
3-10 parts of talcum powder
5-15 parts of porcelain forming auxiliary agent
10-25 parts of plasticizer
0.3-5 parts of stabilizer
1-5 parts of a thermal reversible cross-linking agent.
4. The multi-scale composite thermoreversibly cross-linked ceramizable PVC material as claimed in claim 1, wherein the PVC resin is a PVC resin having a degree of polymerization of 500-2000.
5. The multi-scale composite thermal reversible crosslinked porcelainized PVC material of claim 1, wherein the wollastonite is a wollastonite long fiber, the diameter of the long fiber is 5-10 microns, the length-diameter ratio is 5 ~ 10, and the surface of the long fiber is modified by a coupling agent.
6. The multi-scale composite thermal reversible crosslinking ceramizable PVC material according to claim 1, wherein the montmorillonite is organic intercalation modified nano montmorillonite, the organic modifier is one of Dodecyl Trimethyl Ammonium Bromide (DTAB), hexadecyl trimethyl ammonium bromide (CTAB), Octadecyl Trimethyl Ammonium Bromide (OTAB) and octadecyl dimethyl benzyl ammonium chloride (ODBA), and the particle size of the modified montmorillonite is between 80 ~ 400 nanometers.
7. The multi-scale composite thermoreversible cross-linking ceramizable PVC material according to claim 1, wherein the talc powder is ultrafine talc powder with a particle size of 1-5 μm, and the surface of the talc powder is surface-modified by a coupling agent.
8. The multi-scale composite thermoreversibly cross-linked ceramizable PVC material according to claim 1, wherein the ceramic forming aid is two or three of low melting point lead-free glass powder, zinc borate and chopped glass fiber powder with a melting point of 400 ~ 800 ℃, and the particle size ranges from 10 to 40 microns.
9. The multi-scale composite thermoreversibly cross-linked ceramizable PVC material according to claim 1, wherein the calcium zinc stabilizer is a solid composite calcium-zinc soap stabilizer comprising any of zinc stearate, calcium stearate, zinc laurate and calcium metasilicate.
10. The multi-scale composite thermoreversibly cross-linked ceramizable PVC material according to claim 1, wherein the thermoreversible cross-linking agent is long-chain dibasic tertiary amine, and the chain length of the fat is 5-15 carbon atoms.
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