CN112920470B - Fire-resistant environment-friendly curtain wall and preparation method thereof - Google Patents
Fire-resistant environment-friendly curtain wall and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of building materials, in particular to a fire-resistant environment-friendly curtain wall and a preparation method thereof, wherein the fire-resistant environment-friendly curtain wall is prepared from the following raw materials in parts by weight: 50-60 parts of hydroxypropyl starch, 20-30 parts of filler, 10-15 parts of halloysite nanotube composite flame retardant, 1-2 parts of ammonium polyphosphate, 5-8 parts of polyvinyl alcohol, 1-2 parts of plasticizer, 0.5-1 part of foaming component and 150 parts of water, wherein the halloysite nanotube composite flame retardant is obtained by POSS modification of halloysite nanotubes and deposition of nano inorganic flame-retardant particles on the surface of the halloysite nanotubes, and has the advantages of small density, high mechanical strength, excellent thermal insulation performance, fire resistance, flame retardance and the like, and has wide application prospect.
Description
Technical Field
The invention relates to the field of building materials, in particular to a fire-resistant environment-friendly curtain wall and a preparation method thereof.
Background
The curtain wall is an outer wall enclosure of a building, is not bearing, is a light wall with decorative effect commonly used in modern large and high-rise buildings, consists of a panel and a support structure system, can have certain displacement capacity or certain deformation capacity relative to a main structure, and does not bear the outer enclosure structure or decorative structure of the building (an outer wall frame type support system is also one of curtain wall systems) acted by the main structure; the armor solution is prepared by mixing powders of; wangzhiqian et al, preparation of composite modified starch foaming material by using multi-element foaming agent and performance research [ J ] novel chemical material 2016, 44 (2): 247-: 381-385, but the starch-based foaming material generally has the problems of poor mechanical strength and poor flame retardant property, which hinders further popularization and application.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the development trend, the invention provides a fire-resistant environment-friendly curtain wall and a preparation method thereof.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
a fire-resistant environment-friendly curtain wall is prepared from the following raw materials in parts by weight:
the halloysite nanotube composite flame retardant is obtained by modifying halloysite nanotubes through POSS and depositing nano inorganic flame-retardant particles on the surface of the halloysite nanotubes.
Further, the nano inorganic flame-retardant particles are any one or more of nano antimony trioxide, nano aluminum hydroxide, nano aluminum oxide, nano magnesium hydroxide, nano magnesium oxide, nano antimony pentoxide, nano calcium carbonate, nano titanium dioxide, nano zinc oxide and nano zinc borate.
Further, the nano inorganic flame-retardant particles are nano zinc borate.
Further, the preparation method of the halloysite nanotube composite flame retardant comprises the following steps:
s1: uniformly mixing vinyl trimethoxy silane, methanol and hydrochloric acid, sealing, reacting at room temperature for 20-25 days, filtering, washing a solid with methanol, dissolving with tetrahydrofuran, adding a halloysite nanotube, slowly dropwise adding methanol to enable POSS to grow on the halloysite nanotube, and drying the filtered solid to obtain an intermediate;
s2: heating the intermediate, borax water solution, methanol and modifier to 60-70 deg.C, dropwise adding zinc sulfate water solution, reacting for 5-8 hr, filtering, washing with water, washing with ethanol, and drying.
Further, the modifier is oleic acid or phosphate ester.
Further, the filler is any one or more of sepiolite, coal gangue, montmorillonite, expanded perlite, argil, mica powder, talcum powder, feldspar powder, vermiculite, calcium carbonate, magnesium carbonate, barium sulfate and lithopone.
Further, the plasticizer is N, N-dihydroxyethyl formamide and sorbitol in a mass ratio of 3-5: 1.
Further, the foaming component comprises citric acid, sodium bicarbonate, talcum powder and microcrystalline paraffin, and the mass ratio of the citric acid to the sodium bicarbonate to the talcum powder to the microcrystalline paraffin is 1-2:1-2:1-1.5: 1-1.5.
The preparation method of the fire-resistant environment-friendly curtain wall comprises the following steps:
adding polyvinyl alcohol, hydroxypropyl starch and plasticizer into a high-speed mixer, uniformly mixing at the temperature of 100-120 ℃, adding the mixture into an extruder, extruding, adding the mixture into water, adding filler, halloysite nanotube composite flame retardant, ammonium polyphosphate and foaming components, heating to 70-75 ℃, stirring for 1-3h, injecting the mixture into a mold, drying and curing, foaming the cured material by microwave irradiation for 20-30s at the temperature of 400-800W, and cutting and curing to obtain the fireproof environment-friendly curtain wall.
Further, the water content of the cured material is 13-18%.
The invention has the beneficial effects that:
the hydroxypropyl group in the hydroxypropyl starch can generate steric hindrance effect on one hand, and prevent the aggregation and crystallization of starch chains; on the other hand, the hydroxypropyl can weaken the internal hydrogen bond strength of the starch particle structure, has better expansion and foaming performance, the polyvinyl alcohol has high crystallinity and high density, and can improve the impact resistance, the compression performance and the water and oil resistance of the starch-based material after being added, but because of the existence of a large number of hydroxyl groups in the molecular structure, the polyvinyl alcohol has strong hydrogen bonds in molecules and between molecules, the intermolecular force is extremely large, and the processability is poor, the composite plasticizer is added to form the hydrogen bonds with the polyvinyl alcohol, the hydrogen bonds in the molecules and between the molecules of the polyvinyl alcohol are damaged, the crystalline region is damaged, the compatibility of the processability and the hydroxypropyl starch is improved, the halloysite nanotube is a widely-existing natural clay mineral hollow nanotube, has the advantages of low price, environmental protection, synergistic flame retardance and the like, and the POSS is utilized to modify the halloysite nanotube, the toughness and the dispersibility of the halloysite nanotube can be improved, the heat release rate and the CO generation amount are reduced, the nano zinc borate is used as one of the earliest inorganic flame retardants, the flame-retardant technology is mature, the cost is low, the nano zinc borate is deposited on the tube wall of the halloysite nanotube by using a thermal precipitation method, the nano zinc borate can be flame-retardant in cooperation with the halloysite nanotube, the fire resistance of a curtain wall is further improved, ammonium polyphosphate is safe and environment-friendly, the decomposition temperature is high, the price is low, the flame-retardant and fire-retardant performances can be further improved after the nano zinc borate is added, and the cost is reduced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the fire-resistant environment-friendly curtain wall is prepared from the following raw materials in parts by weight:
55g of hydroxypropyl starch, 20g of expanded perlite, 10g of halloysite nanotube composite flame retardant, 1g of ammonium polyphosphate, 6g of polyvinyl alcohol, 0.75g of N, N-dihydroxyethylformamide, 0.25g of sorbitol, 0.25g of citric acid, 0.25g of sodium bicarbonate, 0.25g of talcum powder, 0.25g of microcrystalline wax and 140g of water.
The preparation method of the halloysite nanotube composite flame retardant comprises the following steps:
uniformly mixing 9mL of vinyl trimethoxy silane, 200mL of methanol and 12mL of hydrochloric acid, sealing, stirring at room temperature for reaction for 20 days, filtering, washing a solid with methanol, dissolving with 50mL of tetrahydrofuran, adding 20g of halloysite nanotube, slowly dropwise adding methanol to grow POSS on the halloysite nanotube, standing for 1h after dropwise adding, drying the filtered solid to obtain an intermediate, heating 20g of the intermediate, 100mL of 0.1mol/L borax water solution, 20mL of methanol and 1mL of oleic acid to 65 ℃, dropwise adding 10mL of 2mol/L zinc sulfate water solution, reacting for 5h after dropwise adding, filtering, washing with water, washing with ethanol, and drying at 80 ℃.
The preparation method of the fire-resistant environment-friendly curtain wall comprises the following steps:
adding polyvinyl alcohol, hydroxypropyl starch, N-dihydroxyethyl formamide and sorbitol into a high-speed mixer, uniformly mixing at 100 ℃, adding the mixture into an extruder, extruding, adding the mixture into water, adding expanded perlite, halloysite nanotube composite flame retardant, ammonium polyphosphate, citric acid, sodium bicarbonate, talcum powder and microcrystalline paraffin, heating to 70 ℃, stirring for 2 hours, injecting the mixture into a mold, drying and curing at 50 ℃ until the water content is 15%, foaming the cured material by microwave irradiation of 400W and 25s, and cutting and curing to obtain the fire-resistant environment-friendly curtain wall.
Example 2:
the fire-resistant environment-friendly curtain wall is prepared from the following raw materials in parts by weight:
60g of hydroxypropyl starch, 20g of expanded perlite, 12g of halloysite nanotube composite flame retardant, 1g of ammonium polyphosphate, 5g of polyvinyl alcohol, 0.75g of N, N-dihydroxyethylformamide, 0.25g of sorbitol, 0.25g of citric acid, 0.25g of sodium bicarbonate, 0.25g of talcum powder, 0.25g of microcrystalline wax and 120g of water.
The preparation method of the halloysite nanotube composite flame retardant comprises the following steps:
uniformly mixing 9mL of vinyl trimethoxy silane, 200mL of methanol and 12mL of hydrochloric acid, sealing, stirring at room temperature to react for 25d, filtering, washing a solid with methanol, dissolving with 50mL of tetrahydrofuran, adding 20g of halloysite nanotube, slowly dropwise adding methanol to grow POSS on the halloysite nanotube, standing for 1h after dropwise adding to obtain an intermediate, taking 20g of the intermediate, 100mL of 0.1mol/L borax aqueous solution, 20mL of methanol and 1mL of oleic acid, heating to 60 ℃, dropwise adding 10mL of 2mol/L zinc sulfate aqueous solution, reacting for 8h after dropwise adding to obtain a reaction product, filtering, washing with ethanol after water washing, and drying at 60 ℃.
The preparation method of the fire-resistant environment-friendly curtain wall comprises the following steps:
adding polyvinyl alcohol, hydroxypropyl starch, N-dihydroxyethyl formamide and sorbitol into a high-speed mixer, uniformly mixing at 110 ℃, adding the mixture into an extruder, extruding, adding the mixture into water, adding expanded perlite, halloysite nanotube composite flame retardant, ammonium polyphosphate, citric acid, sodium bicarbonate, talcum powder and microcrystalline paraffin, heating to 70 ℃, stirring for 1.5h, injecting the mixture into a mold, drying and curing at 50 ℃ until the water content is 13%, and cutting and maintaining the cured material after foaming by microwave irradiation of 800W and 20s to obtain the fire-resistant environment-friendly curtain wall.
Example 3:
the fire-resistant environment-friendly curtain wall is prepared from the following raw materials in parts by weight:
50g of hydroxypropyl starch, 30g of expanded perlite, 10g of halloysite nanotube composite flame retardant, 2g of ammonium polyphosphate, 5g of polyvinyl alcohol, 0.75g of N, N-dihydroxyethylformamide, 0.25g of sorbitol, 0.25g of citric acid, 0.25g of sodium bicarbonate, 0.25g of talcum powder, 0.25g of microcrystalline wax and 120g of water.
The preparation method of the halloysite nanotube composite flame retardant comprises the following steps:
uniformly mixing 9mL of vinyl trimethoxy silane, 200mL of methanol and 12mL of hydrochloric acid, sealing, stirring at room temperature to react for 25d, filtering, washing a solid with methanol, dissolving with 50mL of tetrahydrofuran, adding 20g of halloysite nanotube, slowly dropwise adding methanol to crystallize, allowing POSS to grow on the halloysite nanotube, standing for 1h after dropwise adding to obtain an intermediate, taking 20g of the intermediate, 100mL of 0.1mol/L borax water solution, 20mL of methanol and 1mL of oleic acid, heating to 60 ℃, dropwise adding 10mL of 2mol/L zinc sulfate water solution, reacting for 5h after dropwise adding, filtering, washing with ethanol after water washing, and drying at 80 ℃.
The preparation method of the fire-resistant environment-friendly curtain wall comprises the following steps:
adding polyvinyl alcohol, hydroxypropyl starch, N-dihydroxyethyl formamide and sorbitol into a high-speed mixer, uniformly mixing at 100 ℃, adding the mixture into an extruder, extruding, adding the mixture into water, adding expanded perlite, halloysite nanotube composite flame retardant, ammonium polyphosphate, citric acid, sodium bicarbonate, talcum powder and microcrystalline paraffin, heating to 70 ℃, stirring for 1h, injecting the mixture into a mold, drying and curing at 55 ℃ until the water content is 16%, foaming the cured material by microwave irradiation of 600W and 30s, and cutting and curing to obtain the fire-resistant environment-friendly curtain wall.
Example 4:
the fire-resistant environment-friendly curtain wall is prepared from the following raw materials in parts by weight:
50g of hydroxypropyl starch, 25g of expanded perlite, 15g of halloysite nanotube composite flame retardant, 1g of ammonium polyphosphate, 5g of polyvinyl alcohol, 0.75g of N, N-dihydroxyethylformamide, 0.25g of sorbitol, 0.25g of citric acid, 0.25g of sodium bicarbonate, 0.25g of talcum powder, 0.25g of microcrystalline wax and 150g of water.
The preparation method of the halloysite nanotube composite flame retardant comprises the following steps:
uniformly mixing 9mL of vinyl trimethoxy silane, 200mL of methanol and 12mL of hydrochloric acid, sealing, stirring at room temperature to react for 25d, filtering, washing a solid with methanol, dissolving with 50mL of tetrahydrofuran, adding 20g of halloysite nanotube, slowly dropwise adding methanol to grow POSS on the halloysite nanotube, standing for 1h after dropwise adding to obtain an intermediate, taking 20g of the intermediate, 100mL of 0.1mol/L borax aqueous solution, 20mL of methanol and 1mL of oleic acid, heating to 70 ℃, dropwise adding 10mL of 2mol/L zinc sulfate aqueous solution, reacting for 5h after dropwise adding to obtain a reaction product, filtering, washing with ethanol after water washing, and drying at 65 ℃.
The preparation method of the fire-resistant environment-friendly curtain wall comprises the following steps:
adding polyvinyl alcohol, hydroxypropyl starch, N-dihydroxyethyl formamide and sorbitol into a high-speed mixer, uniformly mixing at 120 ℃, adding the mixture into an extruder, extruding, adding the mixture into water, adding expanded perlite, halloysite nanotube composite flame retardant, ammonium polyphosphate, citric acid, sodium bicarbonate, talcum powder and microcrystalline paraffin, heating to 70 ℃, stirring for 1h, injecting the mixture into a mold, drying and curing at 55 ℃ until the water content is 13%, foaming the cured material by microwave irradiation of 800W and 30s, and cutting and curing to obtain the fire-resistant environment-friendly curtain wall.
Example 5:
the fire-resistant environment-friendly curtain wall is prepared from the following raw materials in parts by weight:
60g of hydroxypropyl starch, 20g of expanded perlite, 15g of halloysite nanotube composite flame retardant, 1g of ammonium polyphosphate, 8g of polyvinyl alcohol, 0.75g of N, N-dihydroxyethylformamide, 0.25g of sorbitol, 0.25g of citric acid, 0.25g of sodium bicarbonate, 0.25g of talcum powder, 0.25g of microcrystalline wax and 130g of water.
The preparation method of the halloysite nanotube composite flame retardant comprises the following steps:
uniformly mixing 9mL of vinyl trimethoxy silane, 200mL of methanol and 12mL of hydrochloric acid, sealing, stirring at room temperature to react for 25d, filtering, washing a solid with methanol, dissolving with 50mL of tetrahydrofuran, adding 20g of halloysite nanotube, slowly dropwise adding methanol to grow POSS on the halloysite nanotube, standing for 1h after dropwise adding, drying the filtered solid to obtain an intermediate, heating 20g of the intermediate, 100mL of 0.1mol/L borax water solution, 20mL of methanol and 1mL of oleic acid to 60 ℃, dropwise adding 10mL of 2mol/L zinc sulfate water solution, reacting for 8h after dropwise adding, filtering, washing with water, washing with ethanol, and drying at 60 ℃.
The preparation method of the fire-resistant environment-friendly curtain wall comprises the following steps:
adding polyvinyl alcohol, hydroxypropyl starch, N-dihydroxyethyl formamide and sorbitol into a high-speed mixer, uniformly mixing at 120 ℃, adding the mixture into an extruder, extruding, adding the mixture into water, adding expanded perlite, halloysite nanotube composite flame retardant, ammonium polyphosphate, citric acid, sodium bicarbonate, talcum powder and microcrystalline paraffin, heating to 70 ℃, stirring for 3 hours, injecting the mixture into a mold, drying and curing at 50 ℃ until the water content is 18%, foaming the cured material by microwave irradiation of 400W and 30s, and cutting and curing to obtain the fire-resistant environment-friendly curtain wall.
Example 6:
the fire-resistant environment-friendly curtain wall is prepared from the following raw materials in parts by weight:
60g of hydroxypropyl starch, 30g of expanded perlite, 15g of halloysite nanotube composite flame retardant, 2g of ammonium polyphosphate, 8g of polyvinyl alcohol, 0.75g of N, N-dihydroxyethylformamide, 0.25g of sorbitol, 0.25g of citric acid, 0.25g of sodium bicarbonate, 0.25g of talcum powder, 0.25g of microcrystalline wax and 150g of water.
The preparation method of the halloysite nanotube composite flame retardant comprises the following steps:
uniformly mixing 9mL of vinyl trimethoxy silane, 200mL of methanol and 12mL of hydrochloric acid, sealing, stirring at room temperature to react for 25d, filtering, washing a solid with methanol, dissolving with 50mL of tetrahydrofuran, adding 20g of halloysite nanotube, slowly dropwise adding methanol to grow POSS on the halloysite nanotube, standing for 1h after dropwise adding, drying the filtered solid to obtain an intermediate, heating 20g of the intermediate, 100mL of 0.1mol/L borax water solution, 20mL of methanol and 1mL of oleic acid to 70 ℃, dropwise adding 10mL of 2mol/L zinc sulfate water solution, reacting for 8h after dropwise adding, filtering, washing with water, washing with ethanol, and drying at 80 ℃.
The preparation method of the fire-resistant environment-friendly curtain wall comprises the following steps:
adding polyvinyl alcohol, hydroxypropyl starch, N-dihydroxyethyl formamide and sorbitol into a high-speed mixer, uniformly mixing at 120 ℃, adding the mixture into an extruder, extruding, adding the mixture into water, adding expanded perlite, halloysite nanotube composite flame retardant, ammonium polyphosphate, citric acid, sodium bicarbonate, talcum powder and microcrystalline paraffin, heating to 75 ℃, stirring for 3 hours, injecting the mixture into a mold, drying and curing at 55 ℃ until the water content is 18%, foaming the cured material by microwave irradiation of 800W and 30s, and cutting and curing to obtain the fire-resistant environment-friendly curtain wall.
Comparative example 1:
essentially the same as example 1 except that the halloysite nanotube composite flame retardant was replaced with halloysite nanotubes.
Comparative example 2:
essentially the same as example 1 except that the halloysite nanotube composite flame retardant was replaced with halloysite nanotubes, POSS, zinc borate.
Comparative example 3:
essentially the same as example 1 except that the halloysite nanotubes did not deposit zinc borate.
The preparation method of the halloysite nanotube composite flame retardant comprises the following steps:
uniformly mixing 9mL of vinyl trimethoxy silane, 200mL of methanol and 12mL of hydrochloric acid, sealing, stirring at room temperature for reaction for 20 days, filtering, washing the solid with methanol, dissolving with 50mL of tetrahydrofuran, adding 20g of halloysite nanotube, slowly dropwise adding methanol to enable POSS to grow on the halloysite nanotube, standing for 1h after dropwise adding is finished, and drying the solid after filtering.
Comparative example 4:
essentially the same as example 1 except that the halloysite nanotubes were not incorporated into POSS.
The preparation method of the halloysite nanotube composite flame retardant comprises the following steps:
heating halloysite nanotube 20g, borax water solution 100mL and 0.1mol/L, methanol 20mL and oleic acid 1mL to 65 ℃, dropwise adding zinc sulfate water solution 10mL and 2mol/L, reacting for 5h after dropwise adding, filtering, washing with water, washing with ethanol, and drying at 80 ℃.
Performance testing
The materials prepared in examples 1 to 6 and comparative examples 1 to 4 of the present invention were subjected to a performance test, wherein the density was tested according to the GB/T6343-2009 standard: the compression strength is tested according to the GB/T8813-2008 standard; the thermal conductivity is tested according to the GB10294-2008 standard: the oxygen index was measured according to GB/T2406-2008, and the results are shown in Table 1:
table 1:
as can be seen from the table 1, the fireproof environment-friendly curtain wall prepared by the method is made of environment-friendly materials, and has the advantages of low density, high mechanical strength, excellent heat insulation performance, fire resistance, flame retardance and wide application prospect.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (6)
1. The fire-resistant environment-friendly curtain wall is characterized by being prepared from the following raw materials in parts by weight:
50-60 parts of hydroxypropyl starch
20-30 parts of filler
10-15 parts of halloysite nanotube composite flame retardant
1-2 parts of ammonium polyphosphate
5-8 parts of polyvinyl alcohol
1-2 parts of plasticizer
0.5-1 part of foaming component
120 portions of water
The halloysite nanotube composite flame retardant is obtained by modifying a halloysite nanotube by POSS and depositing nano inorganic flame-retardant particles on the surface of the halloysite nanotube;
the preparation method of the halloysite nanotube composite flame retardant comprises the following steps:
s1: uniformly mixing vinyl trimethoxy silane, methanol and hydrochloric acid, sealing, reacting at room temperature for 20-25 days, filtering, washing a solid with methanol, dissolving with tetrahydrofuran, adding a halloysite nanotube, slowly dropwise adding methanol to enable POSS to grow on the halloysite nanotube, and drying the filtered solid to obtain an intermediate;
s2: heating the intermediate, a borax water solution, methanol and a modifier to 60-70 ℃, dropwise adding a zinc sulfate water solution, reacting for 5-8h after dropwise adding, filtering, washing with water, washing with ethanol, and drying;
the modifier is oleic acid;
the nano inorganic flame-retardant particles are nano zinc borate.
2. The fire-resistant environment-friendly curtain wall as claimed in claim 1, wherein the filler is any one or more of sepiolite, coal gangue, montmorillonite, expanded perlite, pottery clay, mica powder, talcum powder, feldspar powder, vermiculite, calcium carbonate, magnesium carbonate, barium sulfate and lithopone.
3. The fire-resistant environment-friendly curtain wall as claimed in claim 1, wherein the plasticizer is N, N-dihydroxyethyl formamide and sorbitol in a mass ratio of 3-5: 1.
4. The fire-resistant environment-friendly curtain wall as claimed in claim 1, wherein the foaming component consists of citric acid, sodium bicarbonate, talcum powder and microcrystalline paraffin, and the mass ratio of the citric acid to the sodium bicarbonate to the talcum powder to the microcrystalline paraffin is 1-2:1-2:1-1.5: 1-1.5.
5. The method for preparing the fire-resistant environment-friendly curtain wall as claimed in any one of claims 1 to 4, is characterized by comprising the following steps:
adding polyvinyl alcohol, hydroxypropyl starch and plasticizer into a high-speed mixer, uniformly mixing at the temperature of 100-120 ℃, adding the mixture into an extruder, extruding, adding the mixture into water, adding the filler, the halloysite nanotube composite flame retardant, ammonium polyphosphate and the foaming component, heating to 70-75 ℃, stirring for 1-3h, injecting the mixture into a mold, drying and curing, foaming the cured material by microwave irradiation of 400-800W for 20-30s, and cutting and curing to obtain the fireproof environment-friendly curtain wall.
6. The method for preparing the fire-resistant environment-friendly curtain wall as claimed in claim 5, wherein the water content of the cured material is 13-18%.
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