CN104448389A - CTAB-phosphate flame retardant, composite flame retardant material of CTAB-phosphate flame retardant and preparation method of CTAB-phosphate flame retardant - Google Patents
CTAB-phosphate flame retardant, composite flame retardant material of CTAB-phosphate flame retardant and preparation method of CTAB-phosphate flame retardant Download PDFInfo
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Abstract
The invention belongs to the technical field of novel materials, and particularly relates a CTAB-phosphate flame retardant, a composite flame retardant material of the CTAB-phosphate flame retardant and a preparation method of the CTAB-phosphate flame retardant. The flame retardant is prepared from the following components according to the amount of substance: 1.0-1.5 of aluminum oxide, 1.0-2.0 of inorganic salt, 0.2-0.5 of CTAB, 0.1-0.2 of tetraethylammonium hydroxide and the balance of water. The flame retardant is simple in preparation process, the polymer composite flame retardant material prepared by the flame retardant has good flame retardant performance and good mechanical performance, and the processing performance of the composite flame-retardant material is not influenced.
Description
Technical field
The invention belongs to new material technology field, be specifically related to a kind of CTAB-phosphate flame retardants and use composite flame-proof material and the preparation method of this fire retardant.
Background technology
Macromolecular compound is also high molecular polymer, and it is compared with low molecular compound, and molecular weight is very high.Due to this outstanding feature, make it to show distinctive performance: high molecular, snappiness, high viscosity, degree of crystallinity is low, without gaseous state.These features also give macromolecular material (as matrix material, rubber etc.) and have the excellent feature such as high strength, high tenacity, snappiness.Make it to be widely used in the fields such as electric and electronic, structural construction, Building technology, Rail car manufacture.Although they have good mechanical property, workability and chemical stability; But they belong to organic polymer material, there is inflammableness and combustionvelocity is fast and be difficult to the drawback put out.The disaster hidden-trouble brought thus has become the social concern of common concern, and the inflammableness how changing high molecular polymer has become the emphasis of scientific research.
The method that current reduction polymkeric substance inflammableness is taked mainly adds fire retardant in the polymer.Current widely used fire retardant can be divided into Halogen and halogen-free flame-retardant system by its composition, wherein halogen containing flame-retardant due to discharge during burning a large amount of flue dust and poisonous, be corrosive gas, cause topsoil, hinder lifesaving and escape; And metal hydroxides addition is large in halogen-free flame retardants, other performances of material can be affected again; Fire-retardant oligopolymer in addition, good flame retardation effect and low-smoke low-toxicity, but synthesis technique is complicated, and cost is high.In recent years due to the raising of environmental consciousness and the popularization of sustainable development idea, efficient, low toxicity, low cigarette, machinery and good mechanical properties, there is fire safety, the novel flame redundant material of overall performance optimization becomes the trend that flame retardant area develops.
Summary of the invention
In order to solve the problem, the object of the present invention is to provide the CTAB-phosphate flame retardants between a kind of and polymkeric substance with better consistency; Consistency is good, while playing flame retardant effect very well, carries out structure adjusting optimization to the physical and chemical performance of obtained flame-retardant polymkeric substance.
Two of object of the present invention there is provided the preparation method of described CTAB-phosphate flame retardants, and the method is simple.
Three of object of the present invention there is provided the described composite flame-proof material containing CTAB-phosphate flame retardants, and this composite flame-proof material is efficient, low toxicity, low cigarette not only, and mechanical and good mechanical properties.
Four of object of the present invention there is provided the preparation method of described composite flame-proof material; The method is simple.
The present invention is achieved through the following technical solutions:
CTAB-phosphate flame retardants, is obtained by the following raw material by amount of substance proportioning:
Wherein, described CTAB-phosphate flame retardants is stratiform or mesoporous shape, and CTAB is cetyl trimethylammonium bromide.Stratiform or mesoporous shape, well can improve the consistency between CTAB-phosphate flame retardants and polymkeric substance.The inorganic salt of stratiform are through intercalation processing, interlamellar spacing increases, even in stripping state to a certain degree, this contributes to inorganic skeleton acidic site and macromolecule matrix fully acts on, by catalytic dehydration, be cross-linked into charcoal, make expansion carbon-coating form stable silicate-charcoal barrier layer, thus matter and hot diffusion in obstruct combustion processes, thus improve the heat-resisting oxidation capacity of system.Mesoporous material is developed so far, mostly concentrate on the classics (absorption of Vaculating antigen material, catalysis etc.) and non-classical (medicine controlled releasing, the functional assembly bodies such as responsive polymer) research of performance, in skeleton, Jie of less stable sees phase (this class formation is deviate from back skeleton in lamina membranacea agent (completely) and subsided, coexist with inorganic skeleton and organic lamina membranacea agent complex form, and be situated between see in order) applied research need further to be carried out, and this kind of material stratiform inorganic skeleton and organic lamina membranacea agent intercalation coexist, without the need to further intercalation modifying, simplification of flowsheet.
Preferably, described inorganic salt are the nano phosphate of Fe, Zn, Ti, Mn, Mo, Cu, Ni, Zr, Y, Ce, La.Regulate phosphatic surface acidity by the doping of metal ion, make CTAB-phosphate flame retardants and polymkeric substance have good consistency and is formed surperficial to have the organic-inorganic phosphate of suitable acid sites to be situated between to see self-assembly system.
Preferably, described phosphoric acid salt to be volume percent be 80% nano phosphate.
Preferably, described CTAB to be volume percent be 25% cetyl trimethylammonium bromide.
Prepare the method for described CTAB-phosphate flame retardants, concrete:
A. mix:
First the aluminum oxide of described amount and phosphoric acid are joined in reactor, stir 0.5 ~ 1.5 hour, add cetyl trimethylammonium bromide again, continue stirring 0.5 ~ 1.5 hour, then add halogen, stir 0.5 ~ 1.5 hour, then slowly drip tetraethyl ammonium hydroxide, adjust ph is 7, obtains mixture;
B. react:
The reactor filling described mixture in steps A is heated to 50 ~ 80 DEG C, stirring reaction 20 ~ 25 hours, obtained resultant of reaction;
C. aftertreatment:
Gained resultant of reaction in step B is carried out suction filtration, washing, drying, ball milling, obtained described CTAB-phosphate flame retardants.
Preferably, described halogen is the hydrochloride of Fe, Zn, Ti, Mn, Mo, Cu, Ni, Zr, Y, Ce, La.
A composite flame-proof material containing CTAB-phosphate flame retardants, is obtained by the following raw material calculated by mass parts:
Wherein, institute's fire retardant is described CTAB-phosphate flame retardants.
Preferably, described masterbatch is the one or more combination thing in PE, PP, PS, PVC, ABS, EVA.
Preferably, the mass percentage of described CTAB-phosphate flame retardants in described composite flame-proof material is 1 ~ 10%; The mass ratio of described PP-g-MA and PA6 is 3:2.
Prepare the method for described composite flame-proof material, be specially:
The temperature controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, and screw speed is 12r/min; First PP-g-MA and PA6 is mixed with described amount ratio, and then mix by described amount ratio with CTAB-phosphate flame retardants, use twin screw extruder extruding pelletization, obtained micelle; Finally by obtained micelle and masterbatch extruding pelletization again between 200 ~ 225 DEG C, obtain the described composite flame-proof material containing CTAB-phosphate flame retardants.
The present invention includes aluminum oxide, nano inorganic salt, CTAB, tetraethyl ammonium hydroxide and water 300 ~ 350; And by simple preparation method, the final fire retardant material obtaining organic and inorganic mesoscopic structure.Wherein in inorganic skeleton and macromolecular material catalytic dehydrogenation processes, break to form free radical due to carbochain, and Lewis acid potential energy is enough flutterred and is caught free radical and form crosslinking structure, the one-tenth charcoal of Promotion system.FTIR, RS, XPS confirm, VSB-1 promotes that P-OH forms shrink product, simultaneously also catalysis more phosphorus source phosphorylation and incarbonization, and carbon residue layer smooth surface is fine and close, and barrier property is good.
Organic and inorganic Jie sees compound phase and achieves organic carbon source (as lamina membranacea agent/structure directing agent) and collaborative compound that is inorganic laminated, mesh skeleton.By simple preparation, can obtain the MP (organic-inorganic phosphate is situated between and sees self-assembly system) of stratiform or vesicular structure, the MP of stratiform is at structure and charge matching (lamina membranacea agent and inorganic skeleton reach charge matching by hydrogen bond, covalent linkage effect).In MP system, [the AlPO that vertical angles tetrahedron connects
6] with [Si that is connected of vertical angles tetrahedron in MMT (polynite)
2o
6] the lobe relation such as there is, relative to interlayer, in inorganic bone rack-layer, reactive force is comparatively strong, and therefore, in a shear condition, the lamella of stripping has certain integrity, peels off and is dispersed in macromolecule matrix.
In a word, compared with prior art, fire retardant of the present invention not only preparation technology is simple in the present invention, and energy is good and polymer-compatible, make the composite flame-proof material containing this fire retardant fire-retardant efficient, low toxicity, low cigarette, machinery and good mechanical properties, also do not affect the processing characteristics of polymkeric substance simultaneously.
concrete embodiment
Below in conjunction with embodiment, the present invention is described in further detail, understands the present invention to help those skilled in the art.
Embodiment 1
CTAB-Ce
3(PO
4)
2the preparation of fire retardant
According to n (Al
2o
3): n (P
2o
5): n (CTAB): n (H
2o): n (TMAOH): n (CeCl
2)=1.3:1.0:0.35:335:0.12:0.4 ratio, by a certain amount of Al (OH)
3with a certain amount of 85% H
3pO
4join in the there-necked flask of 1000ml, stir 1h, add a certain amount of CTAB, continue to stir 1h, then add a certain amount of CeCl
2, stir 1h, then slowly drip the TMAOH of 25%, adjust ph is 7, and temperature of reaction 70 DEG C, at room temperature stirs 24h, suction filtration, washing, 80 DEG C of dryings, and ball milling becomes the powder of certain particle diameter; Prepared sample is CTAB-Ce
3(PO
4)
2fire retardant.
PE/PA6/CTAB-Ce
3(PO
4)
2the preparation of/IFR composite flame-proof material
Adopt melt intercalated method, the temperature controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, and screw speed is 12r/min.First PP-g-MA 8 parts is mixed with PA6 (char-forming agent) 6 parts, and then and CTAB-Ce
3(PO
4)
25 parts mix, and use twin screw extruder extruding pelletization, then with itself and masterbatch PE 81 parts extruding pelletization again between 200 ~ 225 DEG C; Obtained PE/PA6/CTAB-Ce
3(PO
4)
2/ IFR composite flame-proof material.
Embodiment 2
CTAB-FePO
4the preparation of fire retardant
According to n (Al
2o
3): n (P
2o
5): n (CTAB): n (H
2o): n (TMAOH): n (FeCl
3)=1.0:1.2:0.2:300:0.1:0.2 ratio, by a certain amount of Al (OH)
3with a certain amount of 85% H
3pO
4join in the there-necked flask of 1000ml, stir 0.5h, add a certain amount of CTAB, continue to stir 0.5h, then add a certain amount of FeCl
3, stir 0.5h, then slowly drip the TMAOH of 25%, adjust ph is 7, and temperature of reaction 50 DEG C, at room temperature stirs 20h, suction filtration, and washing, 80 DEG C of dryings, ball milling becomes the powder of certain particle diameter.Prepared sample is CTAB-FePO
4fire retardant.
PS/PA6/CTAB-FePO
4the preparation of/IFR composite flame-proof material
Adopt melt intercalated method, the temperature controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, and screw speed is 12r/min.First PP-g-MA 10 parts is mixed with PA6 (char-forming agent) 5 parts, and then and CTAB-FePO
45 parts mix, and use twin screw extruder extruding pelletization, then with itself and masterbatch PS 80 parts extruding pelletization again between 200 ~ 225 DEG C; Obtained PS/PA6/CTAB-FePO
4/ IFR composite flame-proof material.
Embodiment 3
CTAB-Ni
3pO
4the preparation of fire retardant
According to n (Al
2o
3): n (P
2o
5): n (CTAB): n (H
2o): n (TMAOH): n (NiCl)=1.5:0.8:0.5:350:0.2:0.5 ratio, by a certain amount of Al (OH)
3with a certain amount of 85% H
3pO
4join in the there-necked flask of 1000ml, stir 1.5h, add a certain amount of CTAB, continue to stir 1.5h, then add a certain amount of NiCl, stir 1.5h, then the TMAOH of 25% is slowly dripped, adjust ph is 7, and temperature of reaction 80 DEG C, at room temperature stirs 25h, suction filtration, washing, 80 DEG C of dryings, ball milling becomes the powder of certain particle diameter.Prepared sample is CTAB-Ni
3pO
4fire retardant.
EVA/PA6/CTAB-Ni
3pO
4the preparation of/IFR composite flame-proof material
Adopt melt intercalated method, the temperature controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, and screw speed is 12r/min.First PP-g-MA 30 parts is mixed with PA6 (char-forming agent) 9 parts, and then and CTAB-Ni
3pO
41 part mixes, and uses twin screw extruder extruding pelletization, then with itself and masterbatch EVA60 part extruding pelletization again between 200 ~ 225 DEG C; Obtained EVA/PA6/CTAB-Ni
3pO
4/ IFR composite flame-proof material.
The present invention can not be exhaustive one by one, in order to make the art personnel understand the present invention further, below mainly carry out contrasting and testing with La salt, be not used for restriction the present invention to other interest field.
Embodiment 4
CTAB-LaPO
4the preparation of fire retardant
According to n (Al
2o
3): n (P
2o
5): n (CTAB): n (H
2o): n (TMAOH): n (LaCl
3)=1.3:1.0:0.35:335:0.12:0.4 ratio, by a certain amount of Al (OH)
3with a certain amount of 85% H
3pO
4join in the there-necked flask of 1000ml, stir 1h, add a certain amount of CTAB, continue to stir 1h, then add a certain amount of LaCl
3, stir 1h, then slowly drip the TMAOH of 25%, adjust ph is 7, and temperature of reaction 70 DEG C, at room temperature stirs 24h, suction filtration, and washing, 80 DEG C of dryings, ball milling becomes the powder of certain particle diameter.Prepared sample is CTAB-LaPO
4fire retardant.
PP/PA6/CTAB-LaPO
4the preparation of/IFR composite flame-proof material
Adopt melt intercalated method, the temperature controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, and screw speed is 12r/min.First PP-g-MA 8 parts is mixed with PA6 (char-forming agent) 6.5 parts, and then and CTAB-LaPO
42.5 parts mix, and use twin screw extruder extruding pelletization, then with itself and masterbatch PP83 part extruding pelletization again between 200 ~ 225 DEG C; Obtained PP/PA6/CTAB-LaPO
4/ IFR composite flame-proof material.
Embodiment 5
CTAB-LaPO
4the preparation of fire retardant
According to n (Al
2o
3): n (P
2o
5): n (CTAB): n (H
2o): n (TMAOH): n (LaCl
3)=1.0:1.2:0.2:300:0.1:0.2 ratio, by a certain amount of Al (OH)
3with a certain amount of 85% H
3pO
4join in the there-necked flask of 1000ml, stir 0.5h, add a certain amount of CTAB, continue to stir 0.5h, then add a certain amount of LaCl
3, stir 0.5h, then slowly drip the TMAOH of 25%, adjust ph is 7, and temperature of reaction 50 DEG C, at room temperature stirs 20h, suction filtration, and washing, 80 DEG C of dryings, ball milling becomes the powder of certain particle diameter.Prepared sample is CTAB-LaPO
4fire retardant.
PP/PA6/CTAB-LaPO
4the preparation of/IFR composite flame-proof material
Adopt melt intercalated method, the temperature controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, and screw speed is 12r/min.First PP-g-MA 10 parts is mixed with PA6 (char-forming agent) 5 parts, and then and CTAB-LaPO
45 parts mix, and use twin screw extruder extruding pelletization, then with itself and masterbatch PP 80 parts extruding pelletization again between 200 ~ 225 DEG C; Obtained PP/PA6/CTAB-LaPO
4/ IFR composite flame-proof material.
Embodiment 6
CTAB-LaPO
4the preparation of fire retardant
According to n (Al
2o
3): n (P
2o
5): n (CTAB): n (H
2o): n (TMAOH): n (LaCl
3)=1.5:0.8:0.5:350:0.2:0.5 ratio, by a certain amount of Al (OH)
3with a certain amount of 85% H
3pO
4join in the there-necked flask of 1000ml, stir 1.5h, add a certain amount of CTAB, continue to stir 1.5h, then add a certain amount of LaCl
3, stir 1.5h, then slowly drip the TMAOH of 25%, adjust ph is 7, and temperature of reaction 80 DEG C, at room temperature stirs 25h, suction filtration, and washing, 80 DEG C of dryings, ball milling becomes the powder of certain particle diameter.Prepared sample is CTAB-LaPO
4fire retardant.
PP/PA6/CTAB-LaPO
4the preparation of/IFR composite flame-proof material
Adopt melt intercalated method, the temperature controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, and screw speed is 12r/min.First PP-g-MA 22.5 parts is mixed with PA6 (char-forming agent) 9 parts, and then and CTAB-LaPO
47.5 parts mix, and use twin screw extruder extruding pelletization, then with itself and masterbatch PP60 part extruding pelletization again between 200 ~ 225 DEG C; Obtained PP/PA6/CTAB-LaPO
4/ IFR composite flame-proof material.
Embodiment 7
CTAB-LAPO
4the preparation of fire retardant
According to n (Al
2o
3): n (P
2o
5): n (CTAB): n (H
2o): n (TMAOH): n (LaCl
3)=1.3:1.2:0.4:310:0.2:0.4 ratio, by a certain amount of Al (OH)
3with a certain amount of 85% H
3pO
4join in the there-necked flask of 1000ml, stir 1h, add a certain amount of CTAB, continue to stir 1h, then add a certain amount of LaCl
3, stir 1h, then slowly drip the TMAOH of 25%, adjust ph is 7, and temperature of reaction 60 DEG C, at room temperature stirs 24h, suction filtration, and washing, 80 DEG C of dryings, ball milling becomes the powder of certain particle diameter.Prepared sample is CTAB-LaPO
4fire retardant.
PP/PA6/CTAB-LaPO
4the preparation of/IFR composite flame-proof material
Adopt melt intercalated method, the temperature controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, and screw speed is 12r/min.First PP-g-MA 15 parts is mixed with PA6 (char-forming agent) 8 parts, and then and CTAB-LaPO
410 parts mix, and use twin screw extruder extruding pelletization, then with itself and masterbatch PP 67 parts extruding pelletization again between 200 ~ 225 DEG C, obtained PP/PA6/CTAB-LaPO
4/ IFR composite flame-proof material.
In the present invention, fire retardant also can adopt the methods such as the precipitator method, sol-gel method, circumfluence method, solid reaction process to be prepared.
Above-described embodiment, just preferred embodiment of the present invention, is not used for limiting the scope of the present invention, therefore all equivalences done with the feature described in the claims in the present invention and principle change or modify, and all should be included within the claims in the present invention scope.
Gained composite flame-proof material in obtained specific embodiment 4-7 is mixing with two Kun mixing roll, then be ground into particulate state composite flame-proof material, finally make mark batten for testing its flame retardant properties with injection moulding machine, and other performances of plastics.
Table 1 experimental design formula
As can be seen from the above table: work as CTAB-LaPO
4when content is 5 ~ 6%, its intercalation-extent of exfoliationization is the highest, and dispersed best, tensile strength and shock strength improve 10% and 42.2% respectively, and surplus charcoal rate reaches 7.78 ~ 10.12%, LOI and reaches 22%, and combustion testing reaches the HB level of UL94 standard.In a word, CTAB-LaPO
4interpolation improve flame retardant properties and mechanical property.
Claims (10)
1.CTAB-phosphate flame retardants, is characterized in that, is obtained by the following raw material by amount of substance proportioning:
Wherein, described CTAB-phosphate flame retardants is stratiform or mesoporous shape, and CTAB is cetyl trimethylammonium bromide.
2. CTAB-phosphate flame retardants as claimed in claim 1, it is characterized in that, described inorganic salt are the nano phosphate of Fe, Zn, Ti, Mn, Mo, Cu, Ni, Zr, Y, Ce, La.
3. CTAB-phosphate flame retardants as claimed in claim 1, is characterized in that, described phosphoric acid salt to be volume percent be 80% nano phosphate.
4. CTAB-phosphate flame retardants as claimed in claim 1, is characterized in that, described CTAB to be volume percent be 25% cetyl trimethylammonium bromide.
5. prepare the method for CTAB-phosphate flame retardants described in any one in claim 1-4, it is characterized in that:
A. mix:
First the aluminum oxide of described amount and phosphoric acid are joined in reactor, stir 0.5 ~ 1.5 hour, add cetyl trimethylammonium bromide again, continue stirring 0.5 ~ 1.5 hour, then add halogen, stir 0.5 ~ 1.5 hour, then slowly drip tetraethyl ammonium hydroxide, adjust ph is 7, obtains mixture;
B. react:
The reactor filling described mixture in steps A is heated to 50 ~ 80 DEG C, stirring reaction 20 ~ 25 hours, obtained resultant of reaction;
C. aftertreatment:
Gained resultant of reaction in step B is carried out suction filtration, washing, drying, ball milling, obtained described CTAB-phosphate flame retardants.
6. prepare the method for CTAB-phosphate flame retardants as claimed in claim 5, it is characterized in that, described halogen is the hydrochloride of Fe, Zn, Ti, Mn, Mo, Cu, Ni, Zr, Y, Ce, La.
7. the composite flame-proof material containing CTAB-phosphate flame retardants, is characterized in that, obtained by the following raw material calculated by mass parts:
Wherein, institute's fire retardant is the CTAB-phosphate flame retardants in claim 1-6 described in any one.
8. composite flame-proof material as claimed in claim 7, it is characterized in that, described masterbatch is the one or more combination thing in PE, PP, PS, PVC, ABS, EVA.
9. composite flame-proof material as claimed in claim 7, it is characterized in that, the mass percentage of described CTAB-phosphate flame retardants in described composite flame-proof material is 1 ~ 10%; The mass ratio of described PP-g-MA and PA6 is 3:2.
10. prepare the method for composite flame-proof material described in any one in claim 7-9, it is characterized in that, be specially:
The temperature controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, and screw speed is 12r/min; First PP-g-MA and PA6 is mixed with described amount ratio, and then mix by described amount ratio with CTAB-phosphate flame retardants, use twin screw extruder extruding pelletization, obtained micelle; Finally by obtained micelle and masterbatch extruding pelletization again between 200 ~ 225 DEG C, obtain the described composite flame-proof material containing CTAB-phosphate flame retardants.
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| CN110364787B (en) * | 2019-07-24 | 2020-11-10 | 易航时代(北京)科技有限公司 | Composite corrosion inhibitor electrolyte, application thereof and magnesium air battery |
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