CN104844828B - A kind of preparation method of the inorganic combustion inhibitor of rubber plastic - Google Patents
A kind of preparation method of the inorganic combustion inhibitor of rubber plastic Download PDFInfo
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- CN104844828B CN104844828B CN201510310707.7A CN201510310707A CN104844828B CN 104844828 B CN104844828 B CN 104844828B CN 201510310707 A CN201510310707 A CN 201510310707A CN 104844828 B CN104844828 B CN 104844828B
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Abstract
The present invention discloses a kind of preparation method of the inorganic combustion inhibitor of rubber plastic, belongs to technical field of flame retardant.Step：Aluminium hydroxide micro powder, cationic monomer are mixed with organic solvent, then in N2Protection under, add silane coupler KH 550, be warming up to, reacted, cool filtering after terminating, and filter cake clean with ethanol, drying obtains coupling agent modified aluminium hydroxide micro powder；Coupling agent modified aluminium hydroxide micro powder is added to the water, acrylamide, anionic monomer, organic silicon monomer, magnesium hydroxide powder and initiator are added, in N2Protection under heat up and reacted, cool after terminating, after filtering, filter cake clean with ethanol, drying obtains coating modification aluminium hydroxide micro powder；Coating modification aluminium hydroxide micro powder, terephthalic acid (TPA) zinc, antimony oxide are well mixed, you can.
Description
Technical field
The present invention discloses a kind of preparation method of the inorganic combustion inhibitor of rubber plastic, belongs to technical field of flame retardant.
Background technology
Rubber combustion has common ground for the burning of other materials, but also has special character.Rubber as high polymer material,
Its combustion process is complex, and its ignition temperature is also above general material.After rubber catches fire, its combustion process can generally divide three
Stage.（1）Thermal decomposition：Reach burning point（Different glue kinds have different burning points）, such as NR is 620 DEG C~670 DEG C）Open first afterwards
Begin to soften and melt, be decomposed into low-molecular material.It is visible in this stage flames of anger, it can be considered the prelude of burning.（2）Burning：Thermal decomposition
There is flame with the oxygen vigorous reaction in air in product, and this indicates that burning formally starts.Along with the release of light and heat, produce
New low molecule combustible（Such as CO）Noncombustibles（Such as CO2）And smog.（3）Burn away：This stage can be extended to all
Untill combustible after-flame.Most of glue kind will undergo these three stages, but halogen rubber is possible to only proceed to second stage,
Because the halide hydrogen generated in burning plays supression.
Fire retardant is a species of rubber special assistant, it is adaptable to require fire-retardant rubber.It is some fire-retardant
Agent also has the effect of plasticising and filling concurrently in addition to energy is fire-retardant.It is traditionally divided into inorganic and organic two major class.It is such fire-retardant
Agent commonly has cooling and iris action, and non-combustible.Because its consumption is big, can alkene release combustible concentration.This based flame retardant
It is divided into hydroxide, inorganic salts and metal oxide again, they are non-combustible powder.CN104262726A, which provides one kind, to be used for
Fire retardant combination of neoprene and preparation method thereof, fire retardant combination comprising antimony oxide, antifungin, zinc aluminate and
Magnesium carbonate；Count by weight, the fire retardant combination includes 10~30 parts of antimony oxide, 20~50 parts of antifungin, aluminium
Sour 10~40 parts of zinc, 10~30 parts of magnesium carbonate.But above-mentioned fire retardant is in use, applied to being led after rubber plastic
The problem of rubbery intensity, the tensile property of cause are reduced.
The content of the invention
The purpose of the present invention is：Rubber is strong caused by conventional inorganic combustion inhibitor is solved after applied to rubber plastic
The problem of degree, tensile property are reduced.
Technical scheme：
A kind of preparation method of the inorganic combustion inhibitor of rubber plastic, comprises the following steps：
1st step, by weight, by 20~40 parts of aluminium hydroxide micro powder, 4~8 parts of cationic monomer with 100~300 parts
Organic solvent mixing, then in N2Protection under, add 5~20 parts of silane resin acceptor kh-550, be warming up to 80~90 DEG C, enter
Row reaction, cool filtering after terminating, and filter cake is cleaned with ethanol, dries, obtains coupling agent modified aluminium hydroxide micro powder；
2nd step, by coupling agent modified aluminium hydroxide micro powder add 300~500 parts of water in, add 100~200 parts third
2~4 parts of acrylamide, 5~8 parts of anionic monomer, 2~4 parts of organic silicon monomer, 5~10 parts of magnesium hydroxide powder and initiator,
N2Protection under be warming up to 60~70 DEG C, reacted, after terminating cool, after filtering, filter cake clean with ethanol, drying, obtain
Coating modification aluminium hydroxide micro powder；
3rd step, coating modification aluminium hydroxide micro powder, 10~15 parts of terephthalic acid (TPA) zinc, 5~10 parts of antimony oxide mixed
Close uniform, you can.
In the 1st described step, organic solvent is one or several kinds of mixed in toluene, dichloromethane or acetic acid ethyl ester
Compound.
In the 1st described step, the particle size range of aluminium hydroxide micro powder is at 0.5~5 μm, content >=98%, and specific surface area >=
2m2·g-1。
In the 1st described step, 4~6 hours reaction time.
In the 2nd described step, initiator is selected from azo-bis-isobutyrate hydrochloride, 2,2- azos（2- amidine propanes）Hydrochloride
Or 2,2- azo [2-（2- imidazoline -2- bases）Propane] dihydrochloride.
Described anionic monomer is acrylic acid, maleic acid, ALS, 2- acrylamido -2- methyl-prop sulphurs
One in acid, 2- acryloyl-oxy -2- methyl propane sulfonic acids, acryloyl-oxy butyl sulfonic acid and (2- acryloyl-oxies) iso-amylene sodium sulfonate
Plant or more than one mixture.
Described cationic monomer is acrylyl oxy-ethyl-trimethyl salmiac, methylacryoyloxyethyl trimethyl ammonia chloride
Ammonium, acryloxypropyl trimethyl ammonium chloride, methacryloxypropyl trimethyl ammonium chloride and N, N- dimethyl diallyl
One or more kinds of mixtures in ammonium chloride.
Described organic silicon monomer be methltriethoxysilone, dimethyldiethoxysilane, methyl trichlorosilane,
One or more of mixtures in dimethyldichlorosilane, phenyltriethoxysilane, dimethoxydiphenylsilane.
Beneficial effect
The present invention is by the way that the surface of aluminium hydroxide micro powder is improved, then by the polymerisation of monomer, by hydroxide
Magnesium is coated on its surface, forms cladding microballoon, when this microballoon is used in rubber after being mixed with others flame retardant constituents, can be with
The problem of intensity for efficiently solving elastomeric material declines.
Embodiment
Embodiment 1
1st step, by aluminium hydroxide micro powder, (at 0.5~5 μm, content >=98% compares table to the particle size range of aluminium hydroxide micro powder
Area >=2m2·g-1) 20g, cationic monomer acrylyl oxy-ethyl-trimethyl salmiac 4g and 100g organic solvent acetic acid second
Vinegar is mixed, then in N2Protection under, add silane resin acceptor kh-550 5g, be warming up to 80 DEG C, reaction 4 hours is carried out, after terminating
Cooling filtering, filter cake is cleaned with ethanol, is dried, is obtained coupling agent modified aluminium hydroxide micro powder；
2nd step, coupling agent modified aluminium hydroxide micro powder added in 300g water, add 100g acrylamide, it is cloudy from
Sub- monomer ALS 5g, organic silicon monomer methltriethoxysilone 2g, magnesium hydroxide powder 5g and initiator are even
The NSC 18620 hydrochloride 2g of nitrogen two, in N2Protection under be warming up to 60 DEG C, reacted, after terminating cool, it is clear with ethanol after filtering
Filter wash cake, drying, obtains coating modification aluminium hydroxide micro powder；
3rd step, coating modification aluminium hydroxide micro powder, terephthalic acid (TPA) zinc 10g, antimony oxide 5g be well mixed, i.e.,
Can.
Embodiment 2
1st step, by aluminium hydroxide micro powder, (at 0.5~5 μm, content >=98% compares table to the particle size range of aluminium hydroxide micro powder
Area >=2m2·g-1) 40g, cationic monomer acrylyl oxy-ethyl-trimethyl salmiac 8g and 300g organic solvent acetic acid second
Vinegar is mixed, then in N2Protection under, add silane resin acceptor kh-550 20g, be warming up to 90 DEG C, carry out reaction 6 hours, terminate
Cooling filtering, filter cake is cleaned with ethanol afterwards, is dried, is obtained coupling agent modified aluminium hydroxide micro powder；
2nd step, coupling agent modified aluminium hydroxide micro powder added in 500g water, add 200g acrylamide, it is cloudy from
Sub- monomer ALS 8g, organic silicon monomer methltriethoxysilone 4g, magnesium hydroxide powder 10g and initiator are even
The NSC 18620 hydrochloride 4g of nitrogen two, in N2Protection under be warming up to 70 DEG C, reacted, after terminating cool, it is clear with ethanol after filtering
Filter wash cake, drying, obtains coating modification aluminium hydroxide micro powder；
3rd step, coating modification aluminium hydroxide micro powder, terephthalic acid (TPA) zinc 15g, antimony oxide 10g be well mixed, i.e.,
Can.
Embodiment 3
1st step, by aluminium hydroxide micro powder, (at 0.5~5 μm, content >=98% compares table to the particle size range of aluminium hydroxide micro powder
Area >=2m2·g-1) 30g, cationic monomer acrylyl oxy-ethyl-trimethyl salmiac 5g and 200g organic solvent acetic acid second
Vinegar is mixed, then in N2Protection under, add silane resin acceptor kh-550 12g, be warming up to 85 DEG C, carry out reaction 5 hours, terminate
Cooling filtering, filter cake is cleaned with ethanol afterwards, is dried, is obtained coupling agent modified aluminium hydroxide micro powder；
2nd step, coupling agent modified aluminium hydroxide micro powder added in 400g water, add 150g acrylamide, it is cloudy from
Sub- monomer ALS 6g, organic silicon monomer methltriethoxysilone 3g, magnesium hydroxide powder 6g and initiator are even
The NSC 18620 hydrochloride 3g of nitrogen two, in N2Protection under be warming up to 65 DEG C, reacted, after terminating cool, it is clear with ethanol after filtering
Filter wash cake, drying, obtains coating modification aluminium hydroxide micro powder；
3rd step, coating modification aluminium hydroxide micro powder, terephthalic acid (TPA) zinc 12g, antimony oxide 7g be well mixed, i.e.,
Can.
Reference examples 1
Difference with embodiment 3 is：Anionic monomer is not added in the 2nd step.
1st step, by aluminium hydroxide micro powder, (at 0.5~5 μm, content >=98% compares table to the particle size range of aluminium hydroxide micro powder
Area >=2m2·g-1) 30g, cationic monomer acrylyl oxy-ethyl-trimethyl salmiac 5g and 200g organic solvent acetic acid second
Vinegar is mixed, then in N2Protection under, add silane resin acceptor kh-550 12g, be warming up to 85 DEG C, carry out reaction 5 hours, terminate
Cooling filtering, filter cake is cleaned with ethanol afterwards, is dried, is obtained coupling agent modified aluminium hydroxide micro powder；
2nd step, coupling agent modified aluminium hydroxide micro powder added in 400g water, add 150g acrylamide, organic
Silicon monomer methltriethoxysilone 3g, magnesium hydroxide powder 6g and initiator azo-bis-isobutyrate hydrochloride 3g, in N2's
65 DEG C are warming up under protection, is reacted, cools after terminating, after filtering, filter cake is cleaned with ethanol, dries, obtains coating modification
Aluminium hydroxide micro powder；
3rd step, coating modification aluminium hydroxide micro powder, terephthalic acid (TPA) zinc 12g, antimony oxide 7g be well mixed, i.e.,
Can.
The preparation of sample
100 parts of butadiene-styrene rubber (SBR1502, rubber, former oxygen index (OI) ＜ 20%), after bag roller, adds each embodiment
With 10 parts of the inorganic combustion inhibitor prepared in reference examples, mix, park 1 day, add 1 part of sulphur, 0.5 part of altax.
Sample conditions of vulcanization：145℃×12min
The national standard of measured performance parameter method institute foundation is specific as follows：Oxygen index (OI) presses GB/T 2046 [1] .2-2009
Determine, hardness is determined by GB 3398.2-2008, tensile strength is determined by GB/T 1701-2001, elongation presses GB/T
1701-2001 is determined, and permanent deformation is determined by GB/T 7759-1996, and smoke density is determined by GB/T 8325.2-2008.
| Oxygen index (OI) | Hardness | Tensile strength | Elongation | Permanent deformation | Smoke density | |
| Embodiment 1 | 32% | 68 | 13.1Mpa | 425% | 35% | 42.6 |
| Embodiment 2 | 31% | 69 | 13.3Mpa | 430% | 40% | 43.4 |
| Embodiment 3 | 34% | 70 | 13.9Mpa | 450% | 32% | 41.0 |
| Reference examples 1 | 28% | 65 | 11.6Mpa | 415% | 39% | 43.0 |
As can be seen from the table, the fire retardant that the present invention is provided can have preferable after applied to elastomeric material
Fire resistance, oxygen index (OI) is high.In addition, due to not adding anionic monomer in reference examples 1, it is impossible to on aluminium hydroxide micro powder surface
Cationic monomer polymerize, the covered effect that result in magnesium hydroxide is bad, is finally led after applied to elastomeric material
The hardness and tensile strength of elastomeric material is caused to occur in that decline.
Claims (1)
1. a kind of preparation method of the inorganic combustion inhibitor of rubber plastic, it is characterised in that comprise the following steps：
1st step, by aluminium hydroxide micro powder 30g, cationic monomer acrylyl oxy-ethyl-trimethyl salmiac 5g and 200g it is organic
Solvent ethyl acetate is mixed, then in N2Protection under, add silane resin acceptor kh-550 12g, be warming up to 85 DEG C, carry out reaction 5
Hour, cool filtering after terminating, and filter cake is cleaned with ethanol, dries, obtains coupling agent modified aluminium hydroxide micro powder, described hydrogen-oxygen
Change the particle size range of aluminium micro mist in 0.5~5 μm, content >=98%, specific surface area >=2m2·g-1；
2nd step, by coupling agent modified aluminium hydroxide micro powder add 400g water in, add 150g acrylamide, anion list
Body ALS 6g, organic silicon monomer methltriethoxysilone 3g, magnesium hydroxide powder 6g and initiator azo two
NSC 18620 hydrochloride 3g, in N2Protection under be warming up to 65 DEG C, reacted, after terminating cool, after filtering, filter is cleaned with ethanol
Cake, drying, obtains coating modification aluminium hydroxide micro powder；
3rd step, coating modification aluminium hydroxide micro powder, terephthalic acid (TPA) zinc 12g, antimony oxide 7g be well mixed, you can.
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| CN101638501B (en) * | 2008-07-29 | 2011-08-17 | 比亚迪股份有限公司 | Flame retardant composition and thermoplastic elastomer containing same |
| CN102649830B (en) * | 2012-05-17 | 2013-11-27 | 陕西科技大学 | Preparation method of cation organic silicon modified polyacrylamide |
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Effective date of registration: 20170712 Address after: 515100 Narita deep ditch, Chaonan District, Guangdong, Shantou Applicant after: Shantou Yuanxing Weaving Co.,Ltd. Address before: 644305 Yibin Province, Changning City, the leading town of Sichuan County, the village of the group of 2, No. 105, attached to No. 2 Applicant before: Fu Xingqin |
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