CN103113621B - Intumescent flame retardant, and preparation method and application thereof - Google Patents
Intumescent flame retardant, and preparation method and application thereof Download PDFInfo
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- CN103113621B CN103113621B CN201310052637.0A CN201310052637A CN103113621B CN 103113621 B CN103113621 B CN 103113621B CN 201310052637 A CN201310052637 A CN 201310052637A CN 103113621 B CN103113621 B CN 103113621B
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- expansion type
- type flame
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 75
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 30
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 10
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 7
- 239000000460 chlorine Substances 0.000 claims description 7
- 229910052801 chlorine Inorganic materials 0.000 claims description 7
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 102000004160 Phosphoric Monoester Hydrolases Human genes 0.000 claims description 3
- 108090000608 Phosphoric Monoester Hydrolases Proteins 0.000 claims description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- ZZVUWRFHKOJYTH-UHFFFAOYSA-N diphenhydramine Chemical compound C=1C=CC=CC=1C(OCCN(C)C)C1=CC=CC=C1 ZZVUWRFHKOJYTH-UHFFFAOYSA-N 0.000 claims 7
- 230000000694 effects Effects 0.000 abstract description 8
- 230000002349 favourable effect Effects 0.000 abstract 1
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical compound [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 abstract 1
- 235000011007 phosphoric acid Nutrition 0.000 abstract 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 12
- 229920000139 polyethylene terephthalate Polymers 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 239000002131 composite material Substances 0.000 description 6
- -1 dipentaerythritol phosphoric acid ester Chemical class 0.000 description 4
- PCHPORCSPXIHLZ-UHFFFAOYSA-N diphenhydramine hydrochloride Chemical compound [Cl-].C=1C=CC=CC=1C(OCC[NH+](C)C)C1=CC=CC=C1 PCHPORCSPXIHLZ-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000010189 synthetic method Methods 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000007974 melamines Chemical class 0.000 description 1
- 229940059574 pentaerithrityl Drugs 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 1
Abstract
The invention relates to an intumescent flame retardant. The chemical formula of the intumescent flame retardant is (CH3O)3Si(CH2)m(N.H3PO4)p((CH2)n)q((CH2)nOPO3H2)k, wherein one (CH2)n is arranged between every two adjacent Ns, (CH2)nOPO3H2 is always connected with N, m and n are independently integers of 1-6, p=2<t>-1, q=2<t>-2, k=2<t>, and t is an integer of 1-6. The flame retardant provided by the invention is favorable and adjustable in flame-retardant effect, convenient to produce and wide in application range; and the reaction temperature is 150 DEG C or below.
Description
Technical field
The present invention relates to a kind of fire retardant, be specifically related to a kind of for making expansion type flame retardant of electric wire sheath and preparation method thereof.
Background technology
In China, fire hazard situation allows of no optimist.Most of macromolecular materials belong to inflammable and combustible matl, fast in combustion processes Flame Propagation speed, produce amount of heat, dense smoke and discharge hydrogenchloride, hydrogen fluoride, the toxic gases such as carbon monoxide.Therefore, macromolecular material is carried out to fire-retardantization processing and be more and more subject to people's attention, adding novel low smoke zero halogen fire resistant agent is an important development direction of fire-retardantization of macromolecular material.What application was more at present is exactly the phosphoric melamine salt halogen-free flame retardants of dipentaerythritol phosphoric acid ester, and this fire retardant has good flame retardant resistance to multiple macromolecular material.Application publication number is that the Chinese invention patent of CN102516303A discloses a kind of expansion type flame retardant for cable jacking synthesizing with raw materials such as tetramethylolmethane, trimeric cyanamide, phosphorus oxychloride.Although method productive rate is higher, this expansion type flame retardant synthesis temperature is that more than 200 ℃ industrial production is restricted.Along with the fast development of cable industry, the fire retardant that manufacturing condition is simple, flame retardant effect is good becomes a kind of active demand in the industry.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of expansion type flame retardant.
Another technical problem to be solved by this invention is to provide a kind of preparation method of expansion type flame retardant.
Another technical problem to be solved by this invention is to provide a kind of application of expansion type flame retardant.
For achieving the above object, the technical solution used in the present invention is:
A kind of expansion type flame retardant, its chemical formula is (CH
3o)
3si (CH
2)
m(NH
3pO
4)
p((CH
2)
n)
q((CH
2)
noPO
3h
2)
k, wherein, be separated with (a CH between between two adjacent N
2)
n, and (CH
2)
noPO
3h
2all the time be connected with N, m and n are independently 1 to 6 integer, p=2
t-1, q=2
t-2, k=2
t, t is 1 to 6 integer.
Preferably, described m and n are independently 1 to 3 integer.
Preferably, described t is 1 to 3 integer.
Particularly, its molecular formula is (CH
3o)
3si-(CH
2)
3-N (CH
2cH
2oPO
3h
2)
2h
3pO
4,
A preparation method for described fire retardant, comprises step (1): dialkyl group hydramine and chlorine alkyl trimethoxysilane are reacted in solvent and under 80-150 ℃ of condition; Step (2): by the product of previous step and phosphatase reaction, afterwards through washing, filter, be drying to obtain described fire retardant; Optionally between described step (1) and step (2), carry out step (3), described step (3): by the product of previous step and the reaction of hydroxyl substituting agent, the product after reaction is finished reacts at 80-150 ℃ with described dialkyl group hydramine in solvent.
Further, concrete steps are as follows: step (1): in reaction vessel, add respectively described dialkyl group hydramine, chlorine alkyl trimethoxysilane and toluene, then reaction vessel is heated to be cooled to room temperature after 80-150 ℃, stirring reaction 1-2 hour; Step (2): add appropriate phosphoric acid in the product of previous step, stirring reaction 0.5-1 hour under normal temperature, repeatedly washs with appropriate methyl alcohol afterwards, is drying to obtain described fire retardant after filtration; Optionally between described step (1) and step (2), carry out step (3), described step (3): add thionyl chloride to react at normal temperatures 1-2 hour in the product of previous step, reaction finishes to add respectively described dialkyl group alcohol and toluene to be cooled to room temperature after stirring reaction 1-2 hour at 80-150 ℃ afterwards.
Particularly, the chemical formula of described dialkyl group hydramine is NH ((CH
2)
n) OH)
2, wherein, n is 1 to 6 integer.
Particularly, the chemical formula of described chlorine alkyl trimethoxysilane is
wherein, m is 1 to 6 integer.
Described expansion type flame retardant is in the application of making in electric wire and cable jacket.
Because technique scheme is used, the present invention compared with prior art has following advantages:
(1) flame retardant effect of the synthetic expansion type flame retardant of the present invention is good, and along with the increase of phosphorus content, flame retardant effect also increases thereupon, therefore, in the time of different fire-retardant requirements, can select the fire retardant of different phosphorus contents;
(2) temperature of reaction of the fire retardant, in the present invention is below 150 ℃, and the harsh degree of condition reduces greatly; And simple to operate, be easy to scale operation;
(3) expansion type flame retardant making can be applied to prepares electric wire and cable jacket, this based flame retardant good stability, and addition is few, has good flame retardant effect.
Accompanying drawing explanation
Accompanying drawing 1 is expansion type flame retardant G1 in embodiment 1-3, G2, the synthetic line of G3 and expansion type flame retardant G1, G2, the chemical structural formula of G3.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiment of the invention is elaborated:
Embodiment 1
This example provides a kind of expansion type flame retardant synthetic method, and its concrete steps are as follows:
(1), in reaction vessel, add respectively 2.65g NH (CH
2cH
2oH)
2,
30ml toluene, is then heated to reaction vessel 100 ℃, stirring reaction and is cooled to room temperature after 1 hour.
(2), in the product of step (1), add 8.06g phosphoric acid, stirring reaction 1 hour under normal temperature, afterwards with 4 washings of appropriate methyl alcohol, the dry product G1 of obtaining after filtering, white solid, productive rate 81.5%, 225 ℃ of fusing points, 305 ℃ of decomposition temperatures.
Embodiment 2
This example provides a kind of expansion type flame retardant synthetic method, and its concrete steps are as follows:
(1), in reaction vessel, add respectively 2.65g NH (CH
2cH
2oH)
2,
30ml toluene, is then heated to reaction vessel 100 ℃, stirring reaction and is cooled to room temperature after 1 hour.
(2), in the product of step (1), add 6.79g thionyl chloride to react at normal temperatures 1 hour, reaction adds respectively 5.24g NH (CH after finishing again
2cH
2oH)
2, 30ml toluene stirring reaction at 100 ℃ is cooled to room temperature after 1 hour.
(3), in the product of step (2), add 20.02g phosphoric acid, stirring reaction 1.5 hours under normal temperature, afterwards with 4 washings of appropriate methyl alcohol, the dry product G2 of obtaining after filtering, white solid, productive rate 72.6%, 215 ℃ of fusing points, 295 ℃ of decomposition temperatures.
Embodiment 3
This example provides a kind of expansion type flame retardant synthetic method, and its concrete steps are as follows:
(1), in reaction vessel, add respectively 2.65g NH (CH
2cH
2oH)
2,
30ml toluene, is then heated to reaction vessel 100 ℃, stirring reaction and is cooled to room temperature after 1 hour.
(2), in the product of step (1), add 6.79g thionyl chloride to react at normal temperatures 1 hour, reaction adds respectively 5.24g NH (CH after finishing again
2cH
2oH)
2, 30ml toluene stirring reaction at 100 ℃ is cooled to room temperature after 1 hour.
(3), in the product of step (2), add 13.81g thionyl chloride to react at normal temperatures 1 hour, reaction adds respectively 10.86g NH (CH after finishing again again
2cH
2oH)
2, 30ml toluene stirring reaction at 100 ℃ is cooled to room temperature after 1 hour.
(4), add again 43.81g phosphoric acid to the product of step (3), stirring reaction 2 hours under normal temperature, afterwards with 4 washings of appropriate methyl alcohol, the dry product G3 of obtaining after filtering, white solid, productive rate 63.7%, 205 ℃ of fusing points, 275 ℃ of decomposition temperatures.
Embodiment 4
This example provides a kind of expansion type flame retardant for cable jacking PET (polyethylene terephthalate), and its concrete steps are as follows:
Above-mentioned expansion type flame retardant G1 and polynite (MMT) are according to mass ratio that 12:1 carries out composite, fire retardant after composite is joined to (fire retardant accounts for massfraction 40%) in PET, there is good flame retardant effect, and along with the increase of fire retardant quality, flame retardant properties also increases, and without drip phenomenon, concrete data are in table 1.
The flame retardant properties of table 1. expansion type flame retardant G1 to PET
Wherein oxygen index is less than 21 for inflammable material, and oxygen index has self-extinguishing between 22～26, and oxygen index is greater than 27 for nonflammable material, and vertical combustion method is divided into V-0, V-1, and V-2 Three Estate, V-0 level is the best rank that material can reach.To the judgement criteria of material rate be sample based on vertical placement after ignition source is removed till from the combustion time of putting out.
Embodiment 5
This example provides a kind of expansion type flame retardant for cable jacking PET (polyethylene terephthalate), and its concrete steps are as follows:
Above-mentioned expansion type flame retardant G2 and polynite (MMT) are according to mass ratio that 10:1 carries out composite, fire retardant after composite is joined to (fire retardant accounts for massfraction 30%) in PET, material has good flame retardant effect, and along with the increase of fire retardant quality, flame retardant properties also increases, and without drip phenomenon, concrete data are in table 2.
The flame retardant properties of table 2. expansion type flame retardant G2 to PET
Embodiment 6
This example provides a kind of expansion type flame retardant for cable jacking PET (polyethylene terephthalate), and its concrete steps are as follows:
Above-mentioned expansion type flame retardant G3 and polynite (MMT) are according to mass ratio that 8:1 carries out composite, fire retardant after composite is joined to (fire retardant accounts for massfraction 30%) in PET, material has good flame retardant effect, and along with the increase of fire retardant quality, flame retardant properties also increases, and without drip phenomenon, concrete data are in table 3.
The flame retardant properties of table 3. expansion type flame retardant G3 to PET
Above-described embodiment is only explanation technical conceive of the present invention and feature; its object is to allow person skilled in the art can understand content of the present invention and implement according to this; can not limit the scope of the invention with this; all equivalences that spirit is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.
Claims (9)
1. an expansion type flame retardant, is characterized in that: its chemical formula is (CH
3o)
3si (CH
2)
m(NH
3pO
4)
p((CH
2)
n)
q((CH
2)
noPO
3h
2)
k, wherein, be separated with (a CH between between two adjacent N
2)
n, and (CH
2)
noPO
3h
2all the time be connected with N, m and n are independently 1 to 6 integer, p=2
t-1, q=2
t-2, k=2
t, t is 1 to 6 integer;
The preparation method of described expansion type flame retardant comprises the steps: step (1): dialkyl group hydramine and chlorine alkyl trimethoxysilane are reacted in solvent and under 80-150 ℃ of condition; Step (2): by the product of previous step and phosphatase reaction, afterwards through washing, filter, be drying to obtain described fire retardant; Optionally between described step (1) and step (2), carry out step (3), described step (3): by the product of previous step and the reaction of hydroxyl substituting agent, the product after reaction is finished reacts at 80-150 ℃ with described dialkyl group hydramine in solvent.
2. expansion type flame retardant according to claim 1, is characterized in that: described m and n are independently 1 to 3 integer.
3. expansion type flame retardant according to claim 1, is characterized in that: described t is 1 to 3 integer.
4. according to the expansion type flame retardant described in any one in claims 1 to 3, it is characterized in that: its molecular formula is (CH
3o)
3si-(CH
2)
3-N (CH
2cH
2oPO
3h
2)
2h
3pO
4,
5. a preparation method for fire retardant as claimed in claim 1, is characterized in that: comprise step (1): dialkyl group hydramine and chlorine alkyl trimethoxysilane are reacted in solvent and under 80-150 ℃ of condition; Step (2): by the product of previous step and phosphatase reaction, afterwards through washing, filter, be drying to obtain described fire retardant; Optionally between described step (1) and step (2), carry out step (3), described step (3): by the product of previous step and the reaction of hydroxyl substituting agent, the product after reaction is finished reacts at 80-150 ℃ with described dialkyl group hydramine in solvent.
6. the preparation method of fire retardant according to claim 5: it is characterized in that: concrete steps are as follows: step (1): add respectively described dialkyl group hydramine, chlorine alkyl trimethoxysilane and toluene in reaction vessel, then reaction vessel is heated to be cooled to room temperature after 80-150 ℃, stirring reaction 1-2 hour; Step (2): add appropriate phosphoric acid in the product of previous step, stirring reaction 0.5-1 hour under normal temperature, repeatedly washs with appropriate methyl alcohol afterwards, is drying to obtain described fire retardant after filtration; Optionally between described step (1) and step (2), carry out step (3), described step (3): add thionyl chloride to react at normal temperatures 1-2 hour in the product of previous step, reaction finishes to add respectively described dialkyl group hydramine and toluene to be cooled to room temperature after stirring reaction 1-2 hour at 80-150 ℃ afterwards.
7. according to the preparation method described in claim 5 or 6, it is characterized in that: the chemical formula of described dialkyl group hydramine is NH ((CH
2) nOH)
2, wherein, n is 1 to 6 integer.
8. according to the preparation method described in claim 5 or 6, it is characterized in that: the chemical formula of described chlorine alkyl trimethoxysilane is
wherein, m is 1 to 6 integer.
9. expansion type flame retardant as claimed in claim 1 is in the application of making in electric wire and cable jacket.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310052637.0A CN103113621B (en) | 2013-02-19 | 2013-02-19 | Intumescent flame retardant, and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310052637.0A CN103113621B (en) | 2013-02-19 | 2013-02-19 | Intumescent flame retardant, and preparation method and application thereof |
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| Publication Number | Publication Date |
|---|---|
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| CN103113621B true CN103113621B (en) | 2014-05-28 |
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Families Citing this family (1)
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| DE102012109685A1 (en) * | 2012-10-11 | 2014-04-17 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Process for the conversion of reactive groups to Si-C-bonded residues of silanes while increasing their spatial distance from each other |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0921174A1 (en) * | 1997-12-08 | 1999-06-09 | Tosoh Corporation | Flame retardant and flame retardant resin composition containing it |
-
2013
- 2013-02-19 CN CN201310052637.0A patent/CN103113621B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0921174A1 (en) * | 1997-12-08 | 1999-06-09 | Tosoh Corporation | Flame retardant and flame retardant resin composition containing it |
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