CN109251552A - A kind of halogen-free high flame-retardant sheet mold materials and preparation method - Google Patents
A kind of halogen-free high flame-retardant sheet mold materials and preparation method Download PDFInfo
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- CN109251552A CN109251552A CN201811091984.3A CN201811091984A CN109251552A CN 109251552 A CN109251552 A CN 109251552A CN 201811091984 A CN201811091984 A CN 201811091984A CN 109251552 A CN109251552 A CN 109251552A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2300/00—Characterised by the use of unspecified polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5425—Silicon-containing compounds containing oxygen containing at least one C=C bond
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- Medicinal Chemistry (AREA)
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- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
Abstract
The invention discloses a kind of halogen-free high flame-retardant sheet mold materials and preparation methods, include: 40 parts -100 parts of unsaturated-resin, 30 parts -80 parts of shrinking agent, 1 part of -10 parts of catalyst, 1 part -10 parts of coupling agent, 1 part of -10 parts of auxiliary agent, 200 parts -300 parts of flame-proof modifier and 1 part -10 parts of thickener according to parts by weight.Making material, heat release rate can reach≤45kw/m in combustion2Below, minimum overlooking heat radiation can reach 30kw/m2More than and the performances such as smoke density Ds4≤150/VOF≤300, smoke toxicity CITg≤0.75；Improve flame retardant property, while meeting high mechanical strength, tensile strength >=100MPA, bending strength >=160MPA, impact flexibility >=100KJ/ ㎡, improve railway locomotive built-in material fire safety under the premise of, its application space can be expanded.
Description
Technical field
The present invention relates to railway fire proofing more particularly to a kind of halogen-free high flame-retardant sheet mold materials and preparation methods.
Background technique
With the rapid development of railway systems technology, in order to adapt to this progressive railway built-in fitting flame-retardancy requirements upgrading, mesh
It is preceding for European Union's railway EN45545R1/HL3 highest grade non-halogen flame-retardant and to meet high mechanical strength moulding compound market and still belong to sky
White, there are no producer or scientific research institution, volume production uses this material, can achieve this fire-retardant rank in other words, but at
This especially high 50-1000 member/kg is differed, and is not obtained and is widely applied to market, limits its application space.
Therefore, the prior art needs further improvement and develops.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of halogen-free high flame-retardant sheet mold materials and
Preparation method, to improve the fire safety of railway locomotive built-in material.
In order to solve the above technical problems, the present invention program includes:
A kind of halogen-free high flame-retardant sheet mold materials includes: according to parts by weight
40 parts -100 parts of unsaturated-resin, 30 parts -80 parts of shrinking agent, 1 part -10 parts of catalyst, 1 part -10 parts
Coupling agent, 1 part -10 parts of auxiliary agent, 200 parts -300 parts of flame-proof modifier and 1 part -10 parts of thickener.
The halogen-free high flame-retardant sheet mold materials, wherein according to parts by weight comprising:
56 parts of unsaturated-resin, 44 parts of shrinking agent, 1 part of catalyst, 1 part of coupling agent, 2 parts of auxiliary agent, 230
The flame-proof modifier and 9 parts of thickener of part.
The halogen-free high flame-retardant sheet mold materials, wherein above-mentioned shrinking agent is saturated polyester, and above-mentioned catalyst was
Benzoic acid spy's butyl ester, above-mentioned coupling agent are methacryloxypropyl trimethoxy silane, and above-mentioned auxiliary agent is phosphoric acid polyesters
Thinner, above-mentioned flame-proof modifier are phosphorus-nitrogen containing flame retardant, and above-mentioned thickener is magnesia.
A method of halogen-free high flame-retardant sheet molding compound is prepared using above-mentioned halogen-free high flame-retardant sheet mold materials comprising
Following steps:
A, ingredient
A1, unsaturated-resin and shrinking agent are put into stirred tank according to above-mentioned formula rate, in 20 DEG C of -25 DEG C of conditions
Under be sufficiently stirred 20 minutes；
A2, catalyst is put into step A1, is sufficiently stirred at 27 DEG C or less 5 minutes, then puts into coupling agent again and help
Agent, and be sufficiently stirred -5 minutes 3 minutes；
A3, the aluminium hydroxide that partial size is 20 microns is put into step A2, stir -3 minutes 2 minutes, adding partial size is
10 microns of aluminium hydroxide continues stirring -3 minutes 2 minutes, adds phosphorus-nitrogen containing flame retardant, stirs 2 minutes, adds smoke elimination
Agent is mixed -25 minutes 20 minutes, maintains the temperature at 30 DEG C -35 DEG C, obtain resin paste；
B, it manufactures
B1, the ratio for being 100:2.5 according to weight ratio by above-mentioned resin paste and magnesia paste, are input to online through metering pump
Hybrid system, mixed resin paste are poured into hopper；
B2, adjustment scraper distance are 1.6mm, and cutting glass starts to be coated, and start to soak by machine track infiltration area
Profit；
B3, the resin paste infiltrated is carried out to curing 72 hours at a temperature of 32 DEG C, viscosity is controlled 6000-7000/ ten thousand
It is taken out when cps, the sheet material after being cured；
C, it suppresses
Sheet material after above-mentioned curing is subjected to molding compacting, at 140 DEG C -148 DEG C, pressure controls the control of molding die temperature
11MPA-13MPA, dwell time 60s/mm obtain halogen-free high flame-retardant sheet molding compound.
The present invention provides a kind of halogen-free high flame-retardant sheet mold materials and preparation method to be made using reasonable group mode
Heat release rate can reach≤45kw/m to material in combustion2Below, minimum overlooking heat radiation can reach 30kw/m2More than,
And the performances such as smoke density Ds4≤150/VOF≤300, smoke toxicity CITg≤0.75；The present invention selects new modified phosphorus nitrogen series
Fire retardant cooperates with aluminium hydroxide and antismoke agent, improves flame retardant property, while meeting high mechanical strength, and tensile strength >=
100MPA, bending strength >=160MPA, impact flexibility >=100KJ/ ㎡ reduce the cost of half, are improving in railway locomotive
Under the premise of the fire safety of package material, its application space can be expanded.
Detailed description of the invention
Fig. 1 is the schematic diagram of preparation method in the present invention；
Fig. 2 is the schematic diagram of the rate of heat release of halogen-free high flame-retardant sheet molding compound in the present invention.
Specific embodiment
The present invention provides a kind of halogen-free high flame-retardant sheet mold materials and preparation methods, to make the purpose of the present invention, technology
Scheme and effect are clearer, clear, and the present invention is described in more detail below.It should be appreciated that described herein specific
Embodiment is only used to explain the present invention, is not intended to limit the present invention.
The present invention provides a kind of halogen-free high flame-retardant sheet mold materials and preparation method, according to parts by weight include: 40 parts-
100 parts of unsaturated-resin, 30 parts -80 parts of shrinking agent, 1 part -10 parts of catalyst, 1 part -10 parts of coupling agent, 1 part -
10 parts of auxiliary agent, 200 parts -300 parts of flame-proof modifier and 1 part -10 parts of thickener.
The present invention is most preferably, according to parts by weight comprising: 56 parts of unsaturated-resin, 44 parts of shrinking agent, 1 part
Catalyst, 1 part of coupling agent, 2 parts of auxiliary agent, 230 parts of flame-proof modifier and 9 parts of thickener.
And above-mentioned shrinking agent is saturated polyester, and above-mentioned catalyst is tertiary butyl perbenzoate, and above-mentioned coupling agent is first
Base acryloyloxypropyltrimethoxysilane, above-mentioned auxiliary agent are phosphoric acid polyesters thinner, and above-mentioned flame-proof modifier is phosphorus nitrogen
Flame retardant, above-mentioned thickener are magnesia.
Halogen-free high flame-retardant sheet molding is prepared using above-mentioned halogen-free high flame-retardant sheet mold materials the present invention also provides a kind of
The method of material, as shown in Figure 1 comprising following steps:
Ingredient
A1, unsaturated-resin and shrinking agent are put into stirred tank according to above-mentioned formula rate, in 20 DEG C of -25 DEG C of conditions
Under be sufficiently stirred 20 minutes；
A2, catalyst is put into step A1, is sufficiently stirred at 27 DEG C or less 5 minutes, then puts into coupling agent again and help
Agent, and be sufficiently stirred -5 minutes 3 minutes；
A3, the aluminium hydroxide that partial size is 20 microns, such as ATH-50 are put into step A2, stir -3 minutes 2 minutes, then
The aluminium hydroxide that partial size is 10 microns, such as ATH-10 is added, continues stirring -3 minutes 2 minutes, adds phosphorus-nitrogen containing flame retardant,
Stirring 2 minutes adds antismoke agent, is mixed -25 minutes 20 minutes, maintains the temperature at 30 DEG C -35 DEG C, obtain resin paste；
Manufacture
B1, the ratio for being 100:2.5 according to weight ratio by above-mentioned resin paste and magnesia paste MK35, are input to through metering pump
On-line mixing system, mixed resin paste are poured into hopper；
B2, adjustment scraper distance are 1.6mm, and cutting glass starts to be coated, and start to soak by machine track infiltration area
Profit；
B3, the resin paste infiltrated is carried out to curing 72 hours at a temperature of 32 DEG C, viscosity is controlled 6000-7000/ ten thousand
It is taken out when cps, the sheet material after being cured；
Compacting
Sheet material after above-mentioned curing is subjected to molding compacting, at 140 DEG C -148 DEG C, pressure controls the control of molding die temperature
11MPA-13MPA, dwell time 60s/mm obtain halogen-free high flame-retardant sheet molding compound.
In order to be exemplified below more detailed embodiment and be illustrated with the present invention is further described.
Unsaturated-resin: selection is low viscosity, high potting resin system DSM-P17, system accounting 20-30%；
Shrinking agent: selection is low viscosity, high filler loading capacity system DSM-H2073, system accounting 20-25%；
Catalyst: selection Aksu (peroxidized t-butyl perbenzoate) TBPB-；
Coupling agent: improving binding force between resin and filler and glass, improves intensity；
Auxiliary agent: including thinner, dispersing agent, release agent etc.；
Fire retardant modifying agent: fire retardant needs to carry out moisture content control to it at this stage, it is desirable that and moisture content≤
0.15%, while mutually proportion is aluminium hydroxide: phosphorus-nitrogen containing flame retardant: antismoke agent=190:30:10, while powder between fire retardant
Particle size content control system after 0.7-0.75 coefficient or so just can guarantee mixing can achieve technological operation requirement between material
Thickener: the thickener is MK35.
Such as using the unsaturated-resin of 56kg, the shrinking agent of 44kg, the catalyst of 1kg, the coupling agent of 1kg, 2kg
The thickener of auxiliary agent, the flame-proof modifier of 230kg and 9kg.
Step 1: ingredient
1.) it will be stirred 20 minutes in resin and shrinking agent investment stirred tank according to above-mentioned formula rate, use temperature
Controller control temperature is spent at 20 DEG C -25 DEG C；
2.) catalyst is put into -- stirring 5 minutes, 27 DEG C of temperature of control or less；
3.) investment coupling agent and BYK auxiliary agent stir 3-5 minutes；
4.) flame-proof modifier is prepared, ATH-50 is weighed and amounts to 140kg, be added in resin, stir 2-3 minutes, addition
The ATH-10 of 40kg is added in resin, stirs 2-3 minutes, weighs phosphor nitrogen combustion inhibitor 30kg, is added in resin, stirs 2 minutes,
20kg antismoke agent is weighed, is added in resin, 20-25min is mixed, keeps 30-35 DEG C of resin paste temperature；
Step 2: production
1.) resin paste and MK35 are input to on-line mixing system through metering pump according to 100:2.5 ratio, it is mixed
Resin paste is poured into hopper；
2.) scraper distance 1.6mm is adjusted, cutting glass starts to be coated, and starts to infiltrate by machine track infiltration area；
3.) resin paste infiltrated is subjected to curing 72h at a temperature of 32 DEG C, viscosity is controlled in 6000-7000/ ten thousand cps
When take out；
Step 3: product is suppressed
1.) sheet material after curing is subjected to molding compacting, for the control of molding die temperature at 140-148 DEG C, pressure controls 11-
13MPA, dwell time 60s/mm；
2.) sampling carries out detection mechanical strength and flame retardant property on product, as shown in Figure 2.
Certainly, described above is only that presently preferred embodiments of the present invention is answered the present invention is not limited to enumerate above-described embodiment
When explanation, anyone skilled in the art is all equivalent substitutes for being made, bright under the introduction of this specification
Aobvious variant, all falls within the essential scope of this specification, ought to be by protection of the invention.
Claims (4)
1. a kind of halogen-free high flame-retardant sheet mold materials, is characterized in that, include: according to parts by weight
40 parts -100 parts of unsaturated-resin, 30 parts -80 parts of shrinking agent, 1 part -10 parts of catalyst, 1 part -10 parts of idol
Join agent, 1 part -10 parts of auxiliary agent, 200 parts -300 parts of flame-proof modifier and 1 part -10 parts of thickener.
2. halogen-free high flame-retardant sheet mold materials according to claim 1, which is characterized in that according to parts by weight comprising:
56 parts of unsaturated-resin, 44 parts of shrinking agent, 1 part of catalyst, 1 part of coupling agent, 2 parts of auxiliary agent, 230 parts
Flame-proof modifier and 9 parts of thickener.
3. halogen-free high flame-retardant sheet mold materials according to claim 1, which is characterized in that above-mentioned shrinking agent is that saturation is poly-
Ester, above-mentioned catalyst are tertiary butyl perbenzoate, and above-mentioned coupling agent is methacryloxypropyl trimethoxy silane, above-mentioned
Auxiliary agent is phosphoric acid polyesters thinner, and above-mentioned flame-proof modifier is phosphorus-nitrogen containing flame retardant, and above-mentioned thickener is magnesia.
4. a kind of side for preparing halogen-free high flame-retardant sheet molding compound using halogen-free high flame-retardant sheet mold materials as described in claim 1
Method comprising following steps:
A, ingredient
A1, according to above-mentioned formula rate by unsaturated-resin and shrinking agent investment stirred tank in, under the conditions of 20 DEG C -25 DEG C into
Row is sufficiently stirred 20 minutes；
A2, catalyst is put into step A1, is sufficiently stirred at 27 DEG C or less 5 minutes, then puts into coupling agent and auxiliary agent again, and
It is sufficiently stirred -5 minutes 3 minutes；
A3, the aluminium hydroxide that partial size is 20 microns being put into step A2, being stirred -3 minutes 2 minutes, adding partial size is 10 micro-
The aluminium hydroxide of rice continues stirring -3 minutes 2 minutes, adds phosphorus-nitrogen containing flame retardant, stirs 2 minutes, adds antismoke agent, mixes
Stirring -25 minutes 20 minutes is closed, 30 DEG C -35 DEG C is maintained the temperature at, obtains resin paste；
B, it manufactures
B1, the ratio for being 100:2.5 according to weight ratio by above-mentioned resin paste and magnesia paste, are input to on-line mixing through metering pump
System, mixed resin paste are poured into hopper；
B2, adjustment scraper distance are 1.6mm, and cutting glass starts to be coated, and start to infiltrate by machine track infiltration area；
B3, the resin paste infiltrated is carried out to curing 72 hours at a temperature of 32 DEG C, viscosity is controlled in 6000-7000/ ten thousand cps
It takes out, the sheet material after being cured；
C, it suppresses
Sheet material after above-mentioned curing is subjected to molding compacting, at 140 DEG C -148 DEG C, pressure controls the control of molding die temperature
11MPA-13MPA, dwell time 60s/mm obtain halogen-free high flame-retardant sheet molding compound.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811091984.3A CN109251552A (en) | 2018-09-19 | 2018-09-19 | A kind of halogen-free high flame-retardant sheet mold materials and preparation method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811091984.3A CN109251552A (en) | 2018-09-19 | 2018-09-19 | A kind of halogen-free high flame-retardant sheet mold materials and preparation method |
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| CN109251552A true CN109251552A (en) | 2019-01-22 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101457010A (en) * | 2007-12-11 | 2009-06-17 | 天津德昊超微新材料有限公司 | Low smoke halogen-free flame retardant ABS resin |
| CN102295798A (en) * | 2010-06-24 | 2011-12-28 | 上海凯波特种电缆料厂有限公司 | Zero-halogen low-smoke flame-retardant injection molding material for branch cable and preparation as well as application thereof |
| CN103232631A (en) * | 2013-06-03 | 2013-08-07 | 北京理工大学 | Halogen-free low-smoke flame-retardant cable sheath material and preparation method of same |
| CN105482399A (en) * | 2015-11-27 | 2016-04-13 | 四川迪弗电工科技有限公司 | Unsaturated polyester resin fiber reinforced sheet-shape molding compound and preparation method thereof |
-
2018
- 2018-09-19 CN CN201811091984.3A patent/CN109251552A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101457010A (en) * | 2007-12-11 | 2009-06-17 | 天津德昊超微新材料有限公司 | Low smoke halogen-free flame retardant ABS resin |
| CN102295798A (en) * | 2010-06-24 | 2011-12-28 | 上海凯波特种电缆料厂有限公司 | Zero-halogen low-smoke flame-retardant injection molding material for branch cable and preparation as well as application thereof |
| CN103232631A (en) * | 2013-06-03 | 2013-08-07 | 北京理工大学 | Halogen-free low-smoke flame-retardant cable sheath material and preparation method of same |
| CN105482399A (en) * | 2015-11-27 | 2016-04-13 | 四川迪弗电工科技有限公司 | Unsaturated polyester resin fiber reinforced sheet-shape molding compound and preparation method thereof |
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Application publication date: 20190122 |