CN104031326A - Modified hard crosslinked polyvinyl chloride flame-retardant foam and preparation method thereof - Google Patents
Modified hard crosslinked polyvinyl chloride flame-retardant foam and preparation method thereof Download PDFInfo
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Abstract
The invention discloses modified hard crosslinked polyvinyl chloride flame-retardant foam and a preparation method thereof. The modified hard crosslinked polyvinyl chloride flame-retardant foam is prepared from 90-99 parts by weight of polyvinyl chloride paste resin, 1-10 parts by weight of chlorinated polyvinyl chloride resin, 3-15 parts by weight of a cross-linking agent, 30-70 parts by weight of isocyanate, 9-24 parts by weight of anhydride, 4-8 parts by weight of an azo foaming agent, 2-15 parts by weight of epoxy soybean oil, 2-6 parts by weight of a filling material and 5-30 parts by weight of a fire retardant. Through formula optimization, the modified hard crosslinked polyvinyl chloride flame-retardant foam having a B1 flame-retardant level is prepared. The modified hard crosslinked polyvinyl chloride flame-retardant foam has original excellent properties of the modified hard crosslinked polyvinyl chloride foam and has good flame resistance.
Description
Technical field
The present invention relates to polymer foams field, in particular to a kind of modified hard cross-linked polrvinyl chloride flame-retardant foam and preparation method thereof.
Background technology
Hard crosslinked polyvinyl chloride foam has light-high-strength, the characteristic feature of the structural core such as high-modulus, with respect to other high-performance foams, as polymethacrylimide foam, polyetherimide foam etc. have, cost of manufacture is low, water resistance is high, the good advantage of flame retardant effect, in an increasingly wide range of applications in fields such as boats and ships, wind energy, communications and transportation, sports equipment, aerospace.
About composition of raw materials and the preparation method of hard crosslinked polyvinyl chloride foam, there are many sections of patents to disclose, as US Patent No. 2007/0200266A1 and US2010/0068487, Chinese patent CN101580573A etc.Though the hard crosslinked polyvinyl chloride foam that existing method prepares itself has flame retardant resistance, but flame retardant rating lower (B2 level) is not suitable for being applied to the occasion (as B1 level) that high flame retardant requires.
Summary of the invention
The object of this invention is to provide a kind of modified hard cross-linked polrvinyl chloride flame-retardant foam, this flame-retardant foam good flame retardation effect, can be applied to the occasion (B1 level) that high flame retardant requires.
Research is found, to adding in the formula of modified hard crosslinked polyvinyl chloride foam fire retardant can improve the flame retardant properties of foam, still, the type of fire retardant, especially the consumption of fire retardant and the proportioning of other raw materials, to the flame retardant properties important of final product.Study the relation of flame retardant properties and consumption proportion by lot of experiments, can find out suitable raw material consumption proportion.
For achieving the above object, the present invention takes following technical scheme:
A kind of modified hard cross-linked polrvinyl chloride flame-retardant foam, it is characterized in that counting ratio by following raw materials in parts by weight is prepared from: 90～99 parts of pvc resin paste grades, 1～10 part of chlorinated polyvinyl chloride resin, 3～15 parts of linking agents, 30～70 parts of isocyanic ester, 9～24 parts, acid anhydrides, 4～8 parts of azo foaming agents, 2～15 parts of epoxy soybean oils, 2～6 parts of fillers, 5～30 parts of fire retardants; Wherein:
Described linking agent is selected from cyanacrylate or trimethylolpropane trimethacrylate;
Described isocyanic ester is selected from a kind of of the '-diphenylmethane diisocyanate of carbodiimide-urine ketoimine modification or poly methylene poly phenyl poly isocyanate or two kinds;
Described acid anhydrides is selected from cis-hexanaphthene-1,2-dicarboxylic anhydride or methyl hexahydrophthalic anhydride;
Described whipping agent is the mixture of Cellmic C 121 and Diisopropyl azodicarboxylate, and both weight ratios are 1: 1～1: 5;
Described filler is selected from one or more of hollow glass micropearl, titanium dioxide, carbon nanotube or polynite;
Described fire retardant is selected from one or more of high reactivity phosphoric acid ester, low corrosion phosphoric acid ester, decabromodiphynly oxide, triaryl phosphate, decabrominated dipheny base ethane.High reactivity phosphoric acid ester preferred high reactivity phosphoric acid ester LYCO-P08 or high reactivity phosphoric acid ester MAX-P16, low corrosion phosphoric acid ester is low corrosion phosphoric acid ester LYCO-P30 preferably.
The K value of described pvc resin paste grade is 70～80, and chlorinated polyvinyl chloride resin chlorinity is not less than 64%, and pvc resin paste grade and chlorinated polyvinyl chloride resin weight sum are 100 parts.
The preparation method that another object of the present invention is to provide above-mentioned modified hard crosslinked polyvinyl chloride foam, takes following steps:
(a) under 0.09MPa, the raw material for liquid in described component is mixed by described weight, then the raw material for solid in described component is added in liquid by described weight, stir and within 15～20 minutes, obtain even pasty mixture;
(b) even pasty mixture being poured into the mould of good seal, is to carry out compression molding under 170～180 DEG C and the pressure condition that is 5～30MPa in temperature, and cooling die die sinking, obtains die briquetting;
(c) die briquetting step (b) being obtained is positioned in the sweating room of 90～98 DEG C and foams, and obtains foam;
(d) foam step (c) being obtained is cured to process and obtains modified hard crosslinked polyvinyl chloride foam in the sweating room of 60 DEG C.
Beneficial effect of the present invention is, pass through optimization of C/C composites, prepare the modified hard cross-linked polrvinyl chloride flame-retardant foam with B1 flame retardant rating, this foam had both had original advantageous property of modified hard crosslinked polyvinyl chloride foam, there is again good flame retardant resistance, for this material enter have high flame retardant require occasion opened window.
Embodiment
The present invention will be further described below:
Every part of following formula is 1 kilogram.
Embodiment 1
Recipe ingredient is pressed row weight part ratio composition: 90 parts of the pvc resin paste grades that K value is 70, 10 parts of the chlorinated polyvinyl chloride resins of chlorinity 64%, 3 parts of cyanacrylates, 30 parts of the '-diphenylmethane diisocyanates of carbodiimide-urine ketoimine modification, cis-hexanaphthene-1, 9 parts of 2-dicarboxylic anhydrides, 4 parts, the mixture of Cellmic C 121 and Diisopropyl azodicarboxylate, and Cellmic C 121 is 1: 1 with the ratio of Diisopropyl azodicarboxylate weight, 2 parts of epoxy soybean oils, 2 parts of hollow glass micropearls, 5 parts of high reactivity phosphoric acid ester LYCO-P08 (or high reactivity phosphoric acid ester MAX-P16).
According to formula batching, be under 0.09MPa in vacuum tightness, the raw material for liquid in described component is mixed by described weight, then the raw material for solid in described component is added in liquid by described weight, stir and within 20 minutes, obtain even pasty mixture; The thickener of preparation is filled to the thick steel die of 25mm, after matched moulds, mould is put into the platen-press of 180 DEG C, pressure is under 5MPa, to keep cooling die after 10min, when die temperature die sinking during lower than 60 DEG C, obtains die briquetting; The sweating room that the die briquetting of taking-up is placed in to 90 DEG C foams, and makes foam; By foam aftertreatment 2 days in the sweating room of 60 DEG C, preparing density is 75kg/m
3hard cross-linked polrvinyl chloride flame-retardant foam.Its performance index are as shown in table 1.
Embodiment 2
Recipe ingredient is pressed row weight part ratio composition: 99 parts of the pvc resin paste grades that K value is 80,1 part of the chlorinated polyvinyl chloride resin of chlorinity 68%, 15 parts of trimethylolpropane trimethacrylates, poly methylene poly phenyl poly isocyanate (commercial goods, for mixture) 70 parts, 24 parts of methyl hexahydrophthalic anhydrides, 8 parts, the mixture of Cellmic C 121 and Diisopropyl azodicarboxylate, and Cellmic C 121 is 1: 5 with the ratio of Diisopropyl azodicarboxylate weight, 15 parts of epoxy soybean oils, 6 parts of titanium dioxide, 30 parts of triaryl phosphates.
According to formula batching, be under 0.09MPa in vacuum tightness, the raw material for liquid in described component is mixed by described weight, then the raw material for solid in described component is added in liquid by described weight, stir and within 20 minutes, obtain even pasty mixture; The thickener of preparation is filled to the thick steel die of 25mm, after matched moulds, mould is put into the platen-press of 170 DEG C, pressure is under 30MPa, to keep cooling die after 10min, when die temperature die sinking during lower than 60 DEG C; The sweating room that the die briquetting of taking-up is placed in to 92 DEG C foams, and makes foam; By foam aftertreatment 2 days in the sweating room of 60 DEG C, preparing density is 45kg/m
3hard crosslinked polyvinyl chloride foam.Its performance index are as shown in table 1.
Embodiment 3
Recipe ingredient is pressed row weight part ratio composition: 95 parts of the pvc resin paste grades that K value is 75, 5 parts of the chlorinated polyvinyl chloride resins of chlorinity 70%, 8 parts of trimethylolpropane trimethacrylates, 25 parts of 25 parts of the '-diphenylmethane diisocyanates of carbodiimide-urine ketoimine modification and poly methylene poly phenyl poly isocyanates, 10 parts of methyl hexahydrophthalic anhydrides, 6 parts, the mixture of Cellmic C 121 and Diisopropyl azodicarboxylate, and Cellmic C 121 is 1: 3 with the ratio of Diisopropyl azodicarboxylate weight, 10 parts of epoxy soybean oils, 3 parts of titanium dioxide, 5 parts of carbon nanotubes, low corrosion phosphoric acid ester LYCO-P30 is 15 parts.
According to formula batching, be under 0.09MPa in vacuum tightness, the raw material for liquid in described component is mixed by described weight, then the raw material for solid in described component is added in liquid by described weight, stir and within 15 minutes, obtain even pasty mixture; The thickener of preparation is filled to the thick steel die of 25mm, after matched moulds, mould is put into the platen-press of 175 DEG C, pressure is under 20MPa, to keep cooling die after 10min, when die temperature die sinking during lower than 60 DEG C; The sweating room that the die briquetting of taking-up is placed in to 95 DEG C foams, and makes foam; By foam aftertreatment 2 days in the sweating room of 60 DEG C, preparing density is 60kg/m
3hard crosslinked polyvinyl chloride foam.Its performance index are as shown in table 1.
Embodiment 4
Recipe ingredient is pressed row weight part ratio composition: 92 parts of the pvc resin paste grades that K value is 76, 8 parts of the chlorinated polyvinyl chloride resins of chlorinity 72%, 10 parts of cyanacrylates, 30 parts of 20 parts of the '-diphenylmethane diisocyanates of carbodiimide-urine ketoimine modification and poly methylene poly phenyl poly isocyanates, cis-hexanaphthene-1, 15 parts of 2-dicarboxylic anhydrides, 7 parts, the mixture of Cellmic C 121 and Diisopropyl azodicarboxylate, and Cellmic C 121 is 1: 2 with the ratio of Diisopropyl azodicarboxylate weight, 5 parts of epoxy soybean oils, 3 parts of titanium dioxide, 1 part of polynite, 8 parts of decabromodiphynly oxides.
According to formula batching, be under 0.09MPa in vacuum tightness, the raw material for liquid in described component is mixed by described weight, then the raw material for solid in described component is added in liquid by described weight, stir and within 15 minutes, obtain even pasty mixture; The thickener of preparation is filled to the thick steel die of 25mm, after matched moulds, mould is put into the platen-press of 178 DEG C, pressure is under 25MPa, to keep cooling die after 10min, when die temperature die sinking during lower than 60 DEG C; The sweating room that the die briquetting of taking-up is placed in to 96 DEG C foams, and makes foam; By foam aftertreatment 2 days in the sweating room of 60 DEG C, preparing density is 70kg/m
3hard crosslinked polyvinyl chloride foam.Its performance index are as shown in table 1.
Embodiment 5
Recipe ingredient is pressed row weight part ratio composition: 94 parts of the pvc resin paste grades that K value is 72, 6 parts of the % chlorinated polyvinyl chloride resins of chlorinity 75, 12 parts of cyanacrylates, 40 parts of 10 parts of the '-diphenylmethane diisocyanates of carbodiimide-urine ketoimine modification and poly methylene poly phenyl poly isocyanates, cis-hexanaphthene-1, 20 parts of 2-dicarboxylic anhydrides, 5 parts, the mixture of Cellmic C 121 and Diisopropyl azodicarboxylate, and Cellmic C 121 is 1: 4 with the ratio of Diisopropyl azodicarboxylate weight, 7 parts of epoxy soybean oils, 1 part of hollow glass micropearl, 1 part of titanium dioxide, 1 part of carbon nanotube, 1 part of polynite, 5 parts of 5 parts, decabrominated dipheny base ethane and decabromodiphynly oxides.
According to formula batching, be under 0.09MPa in vacuum tightness, the raw material for liquid in described component is mixed by described weight, then the raw material for solid in described component is added in liquid by described weight, stir and within 15 minutes, obtain even pasty mixture; The thickener of preparation is filled to the thick steel die of 25mm, after matched moulds, mould is put into the platen-press of 172 DEG C, pressure is under 10MPa, to keep cooling die after 10min, when die temperature die sinking during lower than 60 DEG C; The sweating room that the die briquetting of taking-up is placed in to 98 DEG C foams, and makes foam; By foam aftertreatment 2 days in the sweating room of 60 DEG C, preparing density is 90kg/m
3hard crosslinked polyvinyl chloride foam.Its performance index data are as shown in table 1.
Comparative example 1:
Recipe ingredient is pressed row weight part ratio composition: 92 parts of the pvc resin paste grades that K value is 76,8 parts of the chlorinated polyvinyl chloride resins of chlorinity 72%, 10 parts of cyanacrylates, 30 parts of 20 parts of the '-diphenylmethane diisocyanates of carbodiimide-urine ketoimine modification and poly methylene poly phenyl poly isocyanates, cis-hexanaphthene-1,15 parts of 2-dicarboxylic anhydrides, 7 parts, the mixture of Cellmic C 121 and Diisopropyl azodicarboxylate, and Cellmic C 121 is 1: 2 with the ratio of Diisopropyl azodicarboxylate weight, 5 parts of epoxy soybean oils, 4 parts, calcium carbonate.
According to formula batching, be under 0.09MPa in vacuum tightness, the raw material for liquid in described component is mixed by described weight, then the raw material for solid in described component is added in liquid by described weight, stir and within 15 minutes, obtain even pasty mixture; The thickener of preparation is filled to the thick steel die of 25mm, after matched moulds, mould is put into the platen-press of 178 DEG C, pressure is under 25MPa, to keep cooling die after 10min, when die temperature die sinking during lower than 60 DEG C; The sweating room that the die briquetting of taking-up is placed in to 96 DEG C foams, and makes foam; By foam aftertreatment 2 days in the sweating room of 60 DEG C, preparing density is 62kg/m
3hard crosslinked polyvinyl chloride foam.Its performance index are as shown in table 1.
Table 1 illustrates, owing to not using fire retardant in comparative example, compared with the embodiment 3 of close density, mechanical property and the flame retardant properties of embodiment 3 crosslinked polyvinyl chloride foam that obtains are all significantly higher than comparative example.From embodiment 1 to embodiment 5, can find out, along with the density of crosslinked polyvinyl chloride foam that the present invention obtains increases, its stretching, compression, cutting performance improve.In general, because the present invention has adopted fire retardant, the flame retardant effect of the foam that obtains increases, more than can reaching B1 level.Other a large number of experiments show that, under existing material condition, when amount of flame-retardant agent is less than 5 parts or while being greater than 30 parts, flame retardant effect cannot reach B1 level.
The mechanical property of table 1 embodiment 1-5 and comparative example and thermal characteristics
Claims (4)
1. a modified hard cross-linked polrvinyl chloride flame-retardant foam, it is characterized in that counting ratio by following raw materials in parts by weight is prepared from: 90～99 parts of pvc resin paste grades, 1～10 part of chlorinated polyvinyl chloride resin, 3～15 parts of linking agents, 30～70 parts of isocyanic ester, 9～24 parts, acid anhydrides, 4～8 parts of azo foaming agents, 2～15 parts of epoxy soybean oils, 2～6 parts of fillers, 5～30 parts of fire retardants; Wherein:
Described linking agent is selected from cyanacrylate or trimethylolpropane trimethacrylate;
Described isocyanic ester is selected from a kind of of the '-diphenylmethane diisocyanate of carbodiimide-urine ketoimine modification or poly methylene poly phenyl poly isocyanate or two kinds;
Described acid anhydrides is selected from cis-hexanaphthene-1,2-dicarboxylic anhydride or methyl hexahydrophthalic anhydride;
Described whipping agent is the mixture of Cellmic C 121 and Diisopropyl azodicarboxylate, and both weight ratios are 1: 1～1: 5;
Described filler is selected from one or more of hollow glass micropearl, titanium dioxide, carbon nanotube or polynite;
Described fire retardant is selected from one or more of high reactivity phosphoric acid ester, low corrosion phosphoric acid ester, decabromodiphynly oxide, triaryl phosphate, decabrominated dipheny base ethane.
2. modified hard cross-linked polrvinyl chloride flame-retardant foam as claimed in claim 1, the K value that it is characterized in that described pvc resin paste grade is 70～80, chlorinated polyvinyl chloride resin chlorinity is not less than 64%, and pvc resin paste grade and chlorinated polyvinyl chloride resin weight sum are 100 parts.
3. modified hard cross-linked polrvinyl chloride flame-retardant foam as claimed in claim 1, is characterized in that described high reactivity phosphoric acid ester is high reactivity phosphoric acid ester LYCO-P08 or high reactivity phosphoric acid ester MAX-P16, and described low corrosion phosphoric acid ester is low corrosion phosphoric acid ester LYCO-P30.
4. the preparation method of modified hard cross-linked polrvinyl chloride flame-retardant foam as claimed in claim 1, is characterized in that comprising the steps:
(a) under 0.09MPa, the raw material for liquid in described component is mixed by described weight, then the raw material for solid in described component is added in liquid by described weight, stir and within 15～20 minutes, obtain even pasty mixture;
(b) even pasty mixture being poured into the mould of good seal, is to carry out compression molding under 170～180 DEG C and the pressure condition that is 5～30MPa in temperature, and cooling die die sinking, obtains die briquetting;
(c) die briquetting step (b) being obtained is positioned in the sweating room of 90～98 DEG C and foams, and obtains foam;
(d) foam step (c) being obtained is cured to process and obtains modified hard crosslinked polyvinyl chloride foam in the sweating room of 60 DEG C.
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| CN105803766A (en) * | 2016-04-13 | 2016-07-27 | 北京服装学院 | Superfine filament spinning oil agent and preparation method |
| CN107033811A (en) * | 2017-05-05 | 2017-08-11 | 安徽国登管业科技有限公司 | Effective bonding agent of steel plastic compount and preparation method thereof |
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| CN110982196A (en) * | 2019-12-20 | 2020-04-10 | 厦门市兆泰云智能科技有限公司 | Foam fireproof material suitable for charging station |
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| CN107501780A (en) * | 2017-08-02 | 2017-12-22 | 西藏加速工场孵化器有限公司 | Communication pipe plastic tube and preparation method thereof |
| CN107603071A (en) * | 2017-10-18 | 2018-01-19 | 清华大学 | A kind of PVC foamed composites of resinous paint slag and preparation method thereof |
| CN108724885A (en) * | 2018-04-11 | 2018-11-02 | 南安市创培电子科技有限公司 | A kind of production technology of the compound concrete-cored foamed planks of EPS |
| CN110982189A (en) * | 2019-11-13 | 2020-04-10 | 佛山佛塑科技集团股份有限公司 | PVC structural foam and preparation method thereof |
| CN110982189B (en) * | 2019-11-13 | 2021-10-22 | 佛山佛塑科技集团股份有限公司 | PVC structural foam and preparation method thereof |
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| CN113061310A (en) * | 2021-03-25 | 2021-07-02 | 中国科学院长春应用化学研究所 | Crosslinked polyvinyl chloride structural foam material and preparation method thereof |
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Effective date of registration: 20190809 Address after: Room 1127, Xinhai Lian Building, 601 Huaguoshan Avenue, Lianyungang Economic and Technological Development Zone, Jiangsu Province Patentee after: Weisai (Jiangsu) Composite Material Technology Co., Ltd. Address before: 071000, No. 152, No. 41, Huiyang North Street, Xinshi District, Hebei, Baoding Patentee before: Yuan Chuming |