CN103113708A - Flame retardant ABS (Acrylonitrile Butadiene Styrene) and preparation method and product thereof - Google Patents
Flame retardant ABS (Acrylonitrile Butadiene Styrene) and preparation method and product thereof Download PDFInfo
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- CN103113708A CN103113708A CN2013100424663A CN201310042466A CN103113708A CN 103113708 A CN103113708 A CN 103113708A CN 2013100424663 A CN2013100424663 A CN 2013100424663A CN 201310042466 A CN201310042466 A CN 201310042466A CN 103113708 A CN103113708 A CN 103113708A
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Abstract
The invention discloses flame retardant ABS (Acrylonitrile Butadiene Styrene) and a preparation method and a product thereof. The flame retardant ABS comprises the following components in parts by weight: 100 parts of ABS resin, 5-64 parts of flame retardant, 1-60 parts of flame retardant synergist, 0-50 parts of additive, 0-100 parts of stuffing and 0-10 parts of other assistants. The sum of the flame retardant and the flame retardant synergist in parts by weight is 25-65 parts. The flame retardant synergist is ammonium salt containing at least one NH<4+>. The other additives are charring agents and/or stabilizers. According to the invention, through reasonable selection of the flame retardant synergist, the flame retardant efficiency of hypophosphite or alkyl hypophosphite flame retardant can be greatly improved in ABS resin, and the use amount of the hypophosphite or alkyl hypophosphite flame retardant in ABS resin can be greatly reduced, so that ABS can reach a high flame retardant level on the condition that the addition of the flame retardant is low.
Description
Technical field
The present invention relates to the flame retardance of polymer field, particularly a kind of flame-proof ABS and preparation method thereof and goods.
Background technology
In existing flame-retardant modified ABS, in order to satisfy non-halogen requirement, usually and PC prepare alloy, simultaneously, select phosphorous, nitrogen or its compound system.Use now the most general phosphonium flame retardant and composition thereof mainly contain micro encapsulation red phosphorus, phosphoric acid ester, with ammonium polyphosphate as the Intumscent Flame Retardant System of main body etc.These flame-retardant systems are all to realize fire-retardant by solid phase mechanism.Compare with traditional bromo-antimony compositional flame-retardant system, the phosphonium flame retardant of solid phase fire retardant mechanism and compositional flame-retardant system thereof have the low shortcoming of flame retarding efficiency.
Phosphinates is the phosphonium flame retardant that a class can act on gas phase, but has equally the low problem of flame retarding efficiency, and not during the compositional flame-retardant synergist, needing to add a large amount of phosphinates, just can to reach the UL94V-0 level fire-retardant.Patent CN1660857B and CN100348653C disclose the composition of the composite amino-contained ring texture of a kind of alkyl phosphinate fire retarding synergist, although these fire retarding synergists can play synergistic effect to a certain extent, but its synergistic degree is limited, and therefore the consumption of phosphinates is still higher, has greatly increased the cost of fire-retardant combination.
Summary of the invention
Goal of the invention of the present invention is in order to overcome the deficiencies in the prior art, a kind of flame-proof ABS to be provided, and this flame-proof ABS can in the situation that the fire retardant addition is less, reach high flame retardant rating by the choose reasonable to fire retarding synergist.
Another object of the present invention is to provide the preparation method of described flame-proof ABS.
The goods that provide described flame-proof ABS to prepare are provided another object of the present invention.
Above-mentioned purpose of the present invention is achieved by following technical solution:
A kind of flame-proof ABS in the flame-proof ABS of every 100 weight parts, comprises the following component of calculating by weight:
100 parts of ABS resin;
5 ~ 64 parts of fire retardants;
1 ~ 60 part of fire retarding synergist;
0 ~ 50 part of additive;
0 ~ 100 part of filler;
0 ~ 10 part of other auxiliary agent;
Wherein, the weight part sum of described fire retardant and fire retarding synergist is 25 ~ 65 parts;
Described fire retardant has structure shown in formula I:
Wherein, R
1And R
2Can simultaneously or not be hydrogen or alkyl simultaneously, M be Mg, Ca, Al, Sb, Sn, Ge, Ti, Fe, Zr, Zn, Ce, Bi, Sr, Mn, Li, Na, K and/or be protonated nitrogen base, and wherein m is 1,2,3 or 4;
Described fire retarding synergist is for containing at least a NH
4 +Ammonium salt;
Described additive is char-forming agent and/or stablizer.
A kind of flame-proof ABS in the flame-proof ABS of every 100 weight parts, is comprised of the following component of calculating by weight:
100 parts of ABS resin;
5 ~ 64 parts of fire retardants;
1 ~ 60 part of fire retarding synergist;
0 ~ 50 part of additive;
0 ~ 100 part of filler;
0 ~ 10 part of other auxiliary agent;
Wherein, the weight part sum of described fire retardant and fire retarding synergist is 25 ~ 65 parts;
Described fire retardant has structure shown in formula I:
Wherein, R
1And R
2Can simultaneously or not be hydrogen or alkyl simultaneously, M be Mg, Ca, Al, Sb, Sn, Ge, Ti, Fe, Zr, Zn, Ce, Bi, Sr, Mn, Li, Na, K and/or be protonated nitrogen base, and wherein m is 1,2,3 or 4;
Described fire retarding synergist is for containing at least a NH
4 +Ammonium salt;
Described additive is char-forming agent and/or stablizer.
Wherein, described ABS resin is this area ABS resin (being vinyl cyanide, divinyl and cinnamic terpolymer) commonly used, and normally, in ABS resin, vinyl cyanide accounts for 15 ~ 35wt%, and divinyl accounts for 5 ~ 30wt%, and vinylbenzene accounts for 40 ~ 60wt%.
Wherein, described filler is this area filler commonly used, the effect that its effect is normally played enhancing, improved dimensional stability or satisfy some special purposes the performance of ABS, these fillers can be glass fibre, carbon fiber, natural fiber, talcum powder, kaolin, wollastonite, mica, wilkinite, glass microballon, calcium carbonate, barium sulfate etc.
Wherein, described char-forming agent is this area char-forming agent commonly used, its effect is to help matrix resin to form stable, firm charcoal layer in combustion processes, thereby reach oxygen barrier every the fire retardation of matter, described char-forming agent is selected from the mixture of tetramethylolmethane, pentaerythritol ester, linear phenolic aldehyde, Mierocrystalline cellulose etc. or these materials.
Wherein, described stablizer is this area stablizer commonly used, its effect is the stability of composite flame-retardant agent in processing and moulding process of improving time phosphine (phosphorus) hydrochlorate fire retardant and fire retarding synergist composition thereof, and described stablizer is selected from the mixture of magnesium oxide, calcium oxide, aluminum oxide, zinc oxide, manganese oxide, stannic oxide, zinc borate, zinc, zinc hydroxyl stannate etc. or these materials.
Wherein, the weight part of described fire retardant interpolation is 5 ~ 44 parts; The weight part that more preferably adds is 5 ~ 25 parts.
Wherein, the weight part of described fire retarding synergist interpolation is 1 ~ 40 part; The weight part that more preferably adds is 20 ~ 40 parts.
Wherein, described additive weight part is 0 ~ 25 part.
Wherein, the weight part that adds of described glass fibre is 0 ~ 80 part.
Wherein, the weight part that adds of described other auxiliary agents is 0 ~ 5 part.
Wherein, the weight part of described fire retardant is 5 ~ 25 parts; The weight part of fire retarding synergist is 20 ~ 40 parts.
Wherein, the weight part sum of described fire retardant and fire retarding synergist is preferably 33 ~ 45 parts.
Wherein, the heat decomposition temperature of described fire retarding synergist is more than 180 ℃.
Wherein, the negative ion of described fire retarding synergist is SO
4 2-, HSO
4 -, S
2O
7 2-, Br
-, Cl
-, the aliphatic carboxylic acid root of C1 ~ C3 or the aromatic carboxylic acid root of C7 ~ C10.
Wherein, described fire retarding synergist is ammonium sulfate, aluminium ammonium sulfate, ammonium sulfate magnesium, ammonium sulfate zinc, ammonium sulfate calcium, ammonium sulfate iron, monoammonium sulfate, ammonium pyrosulfate, ammonium chloride, brometo de amonio, ammonium formiate, ammonium acetate, propionic acid ammonium, isopropyl acid ammonium, ammonium benzoate, toluylic acid ammonium, ammonium phthalate, m-phthalic acid ammonium, terephthalic acid ammonium, phenylpropionic acid ammonium, 2-methylphenyl acetic acid ammonium, 3-methylphenyl acetic acid ammonium, 4-methylphenyl acetic acid ammonium, 2-ethyl benzoate ammonium, 3-ethyl benzoate ammonium, 4-ethyl benzoate ammonium.
Wherein, described fire retarding synergist is ammonium sulfate, aluminium ammonium sulfate, monoammonium sulfate, ammonium pyrosulfate, ammonium chloride or brometo de amonio.
Wherein, in described fire retardant, R
1And R
2Can simultaneously or not be the alkyl of hydrogen or C1 ~ C6 simultaneously.
Wherein, in described fire retardant, M is Al, Mg, Ca, Zn, Sn or Fe.
wherein, described fire retardant is hypo-aluminum orthophosphate, magnesium hypophosphite, calcium propionate, ferric hypophosphite, diethyl phospho acid aluminium, diethyl phospho acid magnesium, diethyl phospho acid zinc, diethyl phospho acid calcium, diethyl phospho acid iron, dimethyl phospho acid aluminium, dimethyl phospho acid magnesium, dimethyl phospho acid zinc, dimethyl phospho acid calcium, dimethyl phospho acid iron, dipropyl phospho acid aluminium, dibutyl phospho acid aluminium, diamyl phospho acid aluminium, dihexyl phospho acid aluminium, methylethyl phospho acid aluminium, methyl-propyl phospho acid aluminium, methyl butyl phospho acid aluminium, ethyl propyl phospho acid aluminium, ethyl-butyl phospho acid aluminium, monomethyl phospho acid aluminium, single ethyl phospho acid aluminium, single propyl group phospho acid aluminium, monobutyl phospho acid aluminium, single amyl group phospho acid aluminium, single ethylhexyl hypophosphorous acid aluminium, monomethyl phospho acid magnesium, single ethyl phospho acid magnesium, single propyl group phospho acid magnesium, monobutyl phospho acid magnesium, monomethyl phospho acid calcium, single ethyl phospho acid calcium, single propyl group phospho acid calcium, monobutyl phospho acid calcium.
The preparation method of described flame-proof ABS is characterized in that, comprises the steps: in proportion said components to be mixed, and extrudes to obtain under 180 ~ 230 ℃.
The goods of being made by described flame-proof ABS.
Compared with prior art, the present invention has following beneficial effect:
The present invention is by the choose reasonable to fire retarding synergist, can significantly improve hypophosphite or the flame retarding efficiency of alkyl phosphinate fire retardant in ABS resin, greatly reduce the consumption of hypophosphite in ABS resin or alkyl phosphinate fire retardant, therefore can in the situation that the fire retardant addition is less, make ABS reach high flame retardant rating.
Embodiment
Below in conjunction with some embodiments, composite flame-retardant agent of the present invention, preparation method and application thereof are described further.Specific embodiment is for further describing the present invention, non-limiting protection scope of the present invention.
Embodiments of the invention adopt following raw material:
Hypophosphite used in embodiment is available from continent, Wuhan chemical industry;
Dialkylphosphinic salts is available from German Clariant;
Ammonium sulfate is available from Baoqing, Yueyang chemical industry company limited;
Ammonium chloride is available from sea, river, Zhuzhou environmental protection Industrial Co., Ltd.;
Brometo de amonio is available from reaching chemical industry in the Suzhou City;
Ammonium pyrosulfate is available from chemical industry far away company limited in the permanent industry in Beijing;
Aluminium ammonium sulfate is available from Wuhan gold promise chemical industry company limited;
Ammonium formiate is available from Shanghai gold one-tenth chemical industry company limited;
Ammonium benzoate is available from Shanghai gold one-tenth chemical industry company limited;
Linear phenolic aldehyde: PF-204, Huantai County converge chemical industry company limited forever;
Zinc oxide: rubber grade zinc oxide, Weifang dragon reach zinc industry company limited;
ABS-1:3904, the Shanghai Gaoqiao petrochemical industry, rubber content is 12wt%;
ABS-2:ABS D-100, Taiwan state is tall, and rubber content is 28wt%;
Filler: glass fibre, megalith company;
Composition vertical combustion grade criterion: UL-94;
Extrude processing characteristics criterion: in visual inspection extruding pelletization process, whether the material strip of extruding has the situations such as foaming, variable color, surface irregularity to occur, and judges and extrudes processing characteristics according to extruding material strip foaming, variable color, surface roughness.When the situations such as foaming, variable color, surface irregularity do not appear in material strip, extrude processing characteristics for well; During the situations such as the few foaming of material strip appearance, light discolouration, not roughen of surface, extruding processing characteristics decomposes for slight; The slightly situation such as roughen but still can accept the time, extruding processing characteristics is decomposed of less foaming, light discolouration, surface appears in material strip.
Below be illustrated in the mode of specific embodiment, described raw material is weight part.
Embodiment 1 ~ 18 and Comparative Examples 1 ~ 6
Ratio in table 1 ~ 3 records mixes each component, extrudes under 180 ~ 230 ℃, prepares the flame-proof ABS of embodiment 1 ~ 18 and Comparative Examples 1 ~ 6.The test result of its flame retardant properties and processing characteristics is as shown in table 4.
Table 1
Table 2
Table 3
The performance test of embodiment 1 ~ 18 and Comparative Examples 1 ~ 4 is as shown in table 4:
Table 4
From the results shown in Table 4, when adopting existing MCA/MPP not good as the flame retardant effect of fire retarding synergist.As can be seen from Table 4, flame-proof ABS of the present invention can in the situation that the fire retardant addition is few, reach high flame retardant effect by the choose reasonable to fire retardant and fire retarding synergist.
The above is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or equivalent flow process conversion that utilizes description of the present invention to do; or directly or indirectly be used in other relevant technical fields, all in like manner be included in scope of patent protection of the present invention.
Claims (10)
1. a flame-proof ABS, is characterized in that, in described flame-proof ABS, comprises the following component of calculating by weight:
100 parts of ABS resin;
5 ~ 64 parts of fire retardants;
1 ~ 60 part of fire retarding synergist;
0 ~ 50 part of additive;
0 ~ 100 part of filler;
0 ~ 10 part of other auxiliary agent;
Wherein, the weight part sum of described fire retardant and fire retarding synergist is 25 ~ 65 parts;
Described fire retardant has structure shown in formula I:
Wherein, R
1And R
2Can simultaneously or not be hydrogen or alkyl simultaneously, M be Mg, Ca, Al, Sb, Sn, Ge, Ti, Fe, Zr, Zn, Ce, Bi, Sr, Mn, Li, Na, K and/or be protonated nitrogen base, and wherein m is 1,2,3 or 4;
Described fire retarding synergist is for containing at least a NH
4 +Ammonium salt;
Described additive is char-forming agent and/or stablizer.
2. a flame-proof ABS, is characterized in that, in the flame-proof ABS of every 100 weight parts, is comprised of the following component of calculating by weight:
100 parts of ABS resin;
5 ~ 64 parts of fire retardants;
1 ~ 60 part of fire retarding synergist;
0 ~ 50 part of additive;
0 ~ 100 part of filler;
0 ~ 10 part of other auxiliary agent;
Wherein, the weight part sum of described fire retardant and fire retarding synergist is 25 ~ 65 parts;
Described fire retardant has structure shown in formula I:
Wherein, R
1And R
2Can simultaneously or not be hydrogen or alkyl simultaneously, M be Mg, Ca, Al, Sb, Sn, Ge, Ti, Fe, Zr, Zn, Ce, Bi, Sr, Mn, Li, Na, K and/or be protonated nitrogen base, and wherein m is 1,2,3 or 4;
Described fire retarding synergist is for containing at least a NH
4 +Ammonium salt;
Described additive is char-forming agent and/or stablizer.
3. flame-proof ABS as claimed in claim 1 or 2, is characterized in that, the weight part of described fire retardant is 5 ~ 25 parts; The weight part of fire retarding synergist is 20 ~ 40 parts.
4. flame-proof ABS as claimed in claim 1 or 2, is characterized in that, the heat decomposition temperature of described fire retarding synergist is more than 180 ℃.
5. flame-proof ABS as claimed in claim 1 or 2, is characterized in that, the negative ion of described fire retarding synergist is SO
4 2-, HSO
4 -, S
2O
7 2-, Br
-, Cl
-, the aliphatic carboxylic acid root of C1 ~ C3 or the aromatic carboxylic acid root of C7 ~ C10.
6. flame-proof ABS as claimed in claim 1 or 2, it is characterized in that, described fire retarding synergist is ammonium sulfate, aluminium ammonium sulfate, ammonium sulfate magnesium, ammonium sulfate zinc, ammonium sulfate calcium, ammonium sulfate iron, monoammonium sulfate, ammonium pyrosulfate, ammonium chloride, brometo de amonio, ammonium formiate, ammonium acetate, the propionic acid ammonium, the isopropyl acid ammonium, ammonium benzoate, the toluylic acid ammonium, ammonium phthalate, the m-phthalic acid ammonium, the terephthalic acid ammonium, the phenylpropionic acid ammonium, 2-methylphenyl acetic acid ammonium, 3-methylphenyl acetic acid ammonium, 4-methylphenyl acetic acid ammonium, 2-ethyl benzoate ammonium, 3-ethyl benzoate ammonium and/or 4-ethyl benzoate ammonium.
7. flame-proof ABS as claimed in claim 1 or 2, is characterized in that, in described fire retardant, and R
1And R
2Can simultaneously or not be the alkyl of hydrogen or C1 ~ C6 simultaneously.
8. flame-proof ABS as claimed in claim 1 or 2, is characterized in that, described fire retardant is hypo-aluminum orthophosphate, magnesium hypophosphite, calcium propionate, ferric hypophosphite, diethyl phospho acid aluminium, diethyl phospho acid magnesium, diethyl phospho acid zinc, diethyl phospho acid calcium, diethyl phospho acid iron, dimethyl phospho acid aluminium, dimethyl phospho acid magnesium, dimethyl phospho acid zinc, dimethyl phospho acid calcium, dimethyl phospho acid iron, dipropyl phospho acid aluminium, dibutyl phospho acid aluminium, diamyl phospho acid aluminium, dihexyl phospho acid aluminium, methylethyl phospho acid aluminium, methyl-propyl phospho acid aluminium, methyl butyl phospho acid aluminium, ethyl propyl phospho acid aluminium, ethyl-butyl phospho acid aluminium, monomethyl phospho acid aluminium, single ethyl phospho acid aluminium, single propyl group phospho acid aluminium, monobutyl phospho acid aluminium, single amyl group phospho acid aluminium, single ethylhexyl hypophosphorous acid aluminium, monomethyl phospho acid magnesium, single ethyl phospho acid magnesium, single propyl group phospho acid magnesium, monobutyl phospho acid magnesium, monomethyl phospho acid calcium, single ethyl phospho acid calcium, single propyl group phospho acid calcium and/or monobutyl phospho acid calcium.
9. the preparation method of the described flame-proof ABS of claim 1 ~ 8 any one claim, is characterized in that, comprises the steps: in proportion said components to be mixed, and extrudes to obtain under 180～230 ℃.
10. the goods of being made by the described flame-proof ABS of claim 1 ~ 8 any one claim.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015170130A1 (en) | 2014-05-06 | 2015-11-12 | Italmatch Chemicals S.P.A. | Environmental friendly flame retardant moulding compositions based on thermoplastic impact modified styrenic polymers |
| CN105419218A (en) * | 2016-01-18 | 2016-03-23 | 东莞职业技术学院 | Halogen-free flame-retardant reinforced type ABS (acrylonitrile-butadiene-styrene) composite material and preparation method thereof |
| CN105734428A (en) * | 2016-03-14 | 2016-07-06 | 昆山一邦泰汽车零部件制造有限公司 | Preparation method of light vehicle seat frame |
| CN110577698A (en) * | 2019-10-09 | 2019-12-17 | 江苏万纳普新材料科技有限公司 | special halogen-free flame-retardant synergistic functional master batch for PBT resin modification and preparation method thereof |
| CN115427504A (en) * | 2020-10-27 | 2022-12-02 | 株式会社Lg化学 | Resin composition and molded article |
| CN115044161B (en) * | 2022-06-16 | 2023-11-14 | 金发科技股份有限公司 | Flame-retardant ABS material and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746608A (en) * | 2012-07-13 | 2012-10-24 | 济南泰星精细化工有限公司 | Special environmental-friendly halogen-free flame retardant for ABS (acrylonitrile butadiene styrene) resin |
-
2013
- 2013-02-01 CN CN201310042466.3A patent/CN103113708B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746608A (en) * | 2012-07-13 | 2012-10-24 | 济南泰星精细化工有限公司 | Special environmental-friendly halogen-free flame retardant for ABS (acrylonitrile butadiene styrene) resin |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015170130A1 (en) | 2014-05-06 | 2015-11-12 | Italmatch Chemicals S.P.A. | Environmental friendly flame retardant moulding compositions based on thermoplastic impact modified styrenic polymers |
| US10119019B2 (en) | 2014-05-06 | 2018-11-06 | Italmatch Chemicals S.P.A. | Environmental friendly flame retardant moulding compositions based on thermoplastic impact modified styrenic polymers |
| CN105419218A (en) * | 2016-01-18 | 2016-03-23 | 东莞职业技术学院 | Halogen-free flame-retardant reinforced type ABS (acrylonitrile-butadiene-styrene) composite material and preparation method thereof |
| CN105734428A (en) * | 2016-03-14 | 2016-07-06 | 昆山一邦泰汽车零部件制造有限公司 | Preparation method of light vehicle seat frame |
| CN110577698A (en) * | 2019-10-09 | 2019-12-17 | 江苏万纳普新材料科技有限公司 | special halogen-free flame-retardant synergistic functional master batch for PBT resin modification and preparation method thereof |
| CN110577698B (en) * | 2019-10-09 | 2023-04-07 | 江苏万纳普新材料科技有限公司 | Special halogen-free flame-retardant synergistic functional master batch for modifying polyester engineering plastics and preparation method thereof |
| CN115427504A (en) * | 2020-10-27 | 2022-12-02 | 株式会社Lg化学 | Resin composition and molded article |
| CN115044161B (en) * | 2022-06-16 | 2023-11-14 | 金发科技股份有限公司 | Flame-retardant ABS material and preparation method and application thereof |
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|---|---|
| CN103113708B (en) | 2016-04-20 |
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