CN104448389B - CTAB phosphate flame retardants and its composite flame-proof material and preparation method - Google Patents
CTAB phosphate flame retardants and its composite flame-proof material and preparation method Download PDFInfo
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Abstract
The invention belongs to new material technology field, and in particular to a kind of CTAB phosphate flame retardants and its composite flame-proof material and preparation method using the fire retardant；The fire retardant is prepared by aluminum oxide 1.0~1.5, inorganic salts 1.0~2.0, CTAB0.2~0.5, tetraethyl ammonium hydroxide 0.1~0.2 and the water of the amount proportioning by material；Not only preparation technology is simple by the present invention, and fire resistance, the mechanical property of made obtained polymer composite flame-proof material are preferable, while do not influence its processing characteristics also.
Description
Technical field
The invention belongs to new material technology field, and in particular to a kind of CTAB- phosphate flame retardants and its using this is fire-retardant
The composite flame-proof material and preparation method of agent.
Background technology
High-molecular compound is also high molecular polymer, and compared with low molecular compound, molecular weight is very high for it.Due to
This outstanding feature, it is allowed to show distinctive performance：HMW, high resiliency, high viscosity, crystallinity are low, no gaseous.This
A little features also give high polymer material (such as composite, rubber) with excellent spies such as high intensity, high tenacity, high resiliency
Point.It is allowed to be widely used in the fields such as electric and electronic, structural construction, Building technology, vehicle manufacture.Although they have good
Mechanical performance, machinability and chemical stability；But they belong to high-molecular organic material, there is inflammability and burning velocity
The drawbacks of being difficult to put out soon.Thus the disaster hidden-trouble brought has turned into the social concern of common concern, how to change macromolecule
The inflammability of polymer has become the emphasis of scientific research.
The method that polymer inflammability is taken is reduced at present mainly adds fire retardant in the polymer.Currently make extensively
Fire retardant can be divided into halogen and halogen-free flame-retardant system by its composition, and release is substantial amounts of when wherein halogen containing flame-retardant is due to burning
Flue dust and it is poisonous, be corrosive gas, cause atmosphere pollution, hinder lifesaving and escape；And metal hydroxide in halogen-free flame retardants
Thing addition is big, can influence other performances of material again；Other fire-retardant oligomer, good flame retardation effect and low-smoke low-toxicity, still
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, efficiently, low toxicity,
Low cigarette, machinery and good mechanical properties, there is fire safety, the novel flame redundant material of overall performance optimization to turn into flame retardant area
The trend of development.
The content of the invention
In order to solve the above problems, there is preferable compatibility between polymer it is an object of the invention to provide a kind of
CTAB- phosphate flame retardants；Compatibility is good, while flame retardant effect can be played very well, the materialization to obtained flame-retardant polymer
Performance carries out structure adjusting optimization.
The second object of the present invention there is provided the preparation method of the CTAB- phosphate flame retardants, and this method is simply easy
OK.
The third object of the present invention there is provided the composite flame-proof material containing CTAB- phosphate flame retardants, and this is multiple
Close not only efficient, less toxic, the low cigarette of fire proofing, and machinery and good mechanical properties.
The fourth object of the present invention there is provided the preparation method of the composite flame-proof material；This method is simple and easy.
The present invention is achieved through the following technical solutions：
CTAB- phosphate flame retardants, it is made by the following raw material of the amount proportioning by material：
Wherein, the CTAB- phosphate flame retardants are stratiform or mesoporous shape, and CTAB is cetyl trimethylammonium bromide.
Stratiform or mesoporous shape, the compatibility between CTAB- phosphate flame retardants and polymer can be improved well.The inorganic salts warp of stratiform
Intercalation processing, interlamellar spacing increase are crossed, or even in a certain degree of exfoliated state, this contributes to inorganic skeleton acidic site and macromolecule
Matrix fully acts on, and by catalytic dehydration, is cross-linked into charcoal, expansion carbon-coating is formed stable silicate-charcoal barrier layer, so as to hinder
Every the diffusion of matter in combustion process and heat, thus improve the heat-resisting oxidability of system.Mesoporous material is developed so far, and is focused mostly on greatly
In the classics (absorption, catalysis etc.) of Vaculating antigen material and non-classical (functional assembly such as medicine controlled releasing, responsive polymer body) property
Can research, in skeleton Jie of less stable see phase (this class formation diaphragm plate agent it is (complete) deviate from back skeleton collapse, with inorganic
Skeleton and organic diaphragm plate agent complex form coexist, and be situated between see it is orderly) application study need further to be carried out, and this kind of material
Bed of material shape inorganic skeleton and organic diaphragm plate agent intercalation coexist, without further intercalation modifying, simplification of flowsheet.
It is preferred that the inorganic salts are Fe, Zn, Ti, Mn, Mo, Cu, Ni, Zr, Y, Ce, La nano phosphate.Pass through gold
The doping for belonging to ion adjusts phosphatic surface acidity so that CTAB- phosphate flame retardants have preferable compatible with polymer
Property and formed surface have suitable acid centre organic-inorganic phosphate be situated between see self-assembly system.
It is preferred that the nano phosphate that it is 80% that the phosphate, which is percent by volume,.
It is preferred that the cetyl trimethylammonium bromide that it is 25% that the CTAB, which is percent by volume,.
The method for preparing the CTAB- phosphate flame retardants, specifically：
A. mix：
First the aluminum oxide of the amount and phosphoric acid are added in reactor, stirred 0.5~1.5 hour, then adds cetyl
Trimethylammonium bromide, continue stirring 0.5~1.5 hour, be subsequently added into halogen, stir 0.5~1.5 hour, be then slowly added dropwise
Tetraethyl ammonium hydroxide, regulation pH value is 7, obtains mixture；
B. react：
The reactor that the mixture is filled in step A is heated to 50~80 DEG C, stirring reaction 20~25 hours,
Reaction product is made；
C. post-process：
Gained reaction product in step B is filtered, washed, dried, ball milling, the CTAB- phosphate resistance is made
Fire agent.
It is preferred that the halogen is Fe, Zn, Ti, Mn, Mo, Cu, Ni, Zr, Y, Ce, La hydrochloride.
A kind of composite flame-proof material containing CTAB- phosphate flame retardants, is made by the following raw material calculated in parts by mass：
Wherein, institute's fire retardant is described CTAB- phosphate flame retardants.
It is preferred that the masterbatch is the one or more combination thing in PE, PP, PS, PVC, ABS, EVA.
It is preferred that weight/mass percentage composition of the CTAB- phosphate flame retardants in the composite flame-proof material be 1~
10%；The mass ratio of the PP-g-MA and PA6 are 3:2.
The method for preparing the composite flame-proof material, it is specially：
The temperature for controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, screw speed 12r/min；First will
PP-g-MA is mixed with PA6 with the amount ratio, is then well mixed again with CTAB- phosphate flame retardants by the amount ratio, with double
Screw extruder extruding pelletization, micelle is made；Finally by obtained micelle and masterbatch, extrusion is made again between 200~225 DEG C
Grain, is made the 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 pass through letter
Single preparation method, the final fire proofing for obtaining organic and inorganic mesoscopic structure.Wherein inorganic skeleton is catalyzed with high polymer material
In certain embodiments, due to the free radical that breaks to form of carbochain, and lewis acid potential energy is enough flutterred and catches free radical formation cross-linked structure, promotees
Enter system into charcoal.FTIR, RS, XPS confirm that VSB-1 promotes P-OH to form shrink product, while has also been catalyzed more phosphorus sources
Phosphorylation and incarbonization, and the smooth densification of carbon residue layer surface, barrier property are good.
Organic and inorganic Jie, which sees compound phase, realizes organic carbon source (as diaphragm plate agent/structure directing agent) and inorganic laminated, net
The collaboration of shape skeleton is compound.By simply preparing, the MP (organic-inorganic phosphates of stratiform or loose structure can be obtained
It is situated between and sees self-assembly system), (diaphragm plate agent and inorganic skeleton pass through hydrogen bond, covalent bond effect in structure and charge matching by the MP of stratiform
Reach charge matching).In MP systems, [the AlPO of vertical angles tetrahedron connection6] with MMT (montmorillonite) in vertical angles tetrahedron
[the Si of connection2O6] have and wait valve relation, relative to interlayer, in inorganic bone rack-layer, active force is stronger, therefore, in a shear condition,
The lamella of stripping has certain integrality, and stripping is dispersed in macromolecule matrix.
In a word, the present invention compared with prior art, not only preparation technology is simple for fire retardant of the present invention, and can well with
Polymer-compatible, make the composite flame-proof material containing the fire retardant fire-retardant efficient, less toxic, low cigarette, machinery and good mechanical properties,
The processing characteristics of polymer is not influenceed also simultaneously.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, is managed to help those skilled in the art
The solution present invention.
Embodiment 1
CTAB-Ce3(PO4)2The preparation of fire retardant
According to n (Al2O3):n(P2O5):n(CTAB):n(H2O):n(TMAOH):n(CeCl2)=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% H3PO4It is added in 1000ml there-necked flask,
1h is stirred, adds a certain amount of CTAB, continues to stir 1h, adds a certain amount of CeCl2, 1h is stirred, is then slowly added dropwise
25% TMAOH, regulation pH value is 7,70 DEG C of reaction temperature, 24h is stirred at room temperature, and is filtered, washing, 80 DEG C of dryings, ball milling
Into the powder of certain particle diameter；Prepared sample is CTAB-Ce3(PO4)2Fire retardant.
PE/PA6/CTAB-Ce3(PO4)2The preparation of/IFR composite flame-proof materials
Using melt intercalated method, the temperature for controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, and screw speed is
12r/min.8 parts of PP-g-MA is mixed for 6 parts with PA6 (carbon forming agent) first, then again with CTAB-Ce3(PO4)25 parts of mixing
Uniformly, with double screw extruder extruding pelletization, then with its with masterbatch PE 81 parts of extruding pelletizations again between 200~225 DEG C；
PE/PA6/CTAB-Ce is made3(PO4)2/ IFR composite flame-proof materials.
Embodiment 2
CTAB-FePO4The preparation of fire retardant
According to n (Al2O3):n(P2O5):n(CTAB):n(H2O):n(TMAOH):n(FeCl3)=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% H3PO4It is added in 1000ml there-necked flask, stirs
0.5h, a certain amount of CTAB is added, continue to stir 0.5h, add a certain amount of FeCl3, 0.5h is stirred, is then slowly added dropwise
25% TMAOH, regulation pH value is 7,50 DEG C of reaction temperature, 20h is stirred at room temperature, and is filtered, washing, 80 DEG C of dryings, ball milling
Into the powder of certain particle diameter.Prepared sample is CTAB-FePO4Fire retardant.
PS/PA6/CTAB-FePO4The preparation of/IFR composite flame-proof materials
Using melt intercalated method, the temperature for controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, and screw speed is
12r/min.10 parts of PP-g-MA is mixed for 5 parts with PA6 (carbon forming agent) first, then again with CTAB-FePO45 parts of mixing are equal
It is even, with double screw extruder extruding pelletization, then with its with masterbatch PS 80 parts of extruding pelletizations again between 200~225 DEG C；System
Obtain PS/PA6/CTAB-FePO4/ IFR composite flame-proof materials.
Embodiment 3
CTAB-Ni3PO4The preparation of fire retardant
According to n (Al2O3):n(P2O5):n(CTAB):n(H2O):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% H3PO4It is added in 1000ml there-necked flask, stirs
1.5h, a certain amount of CTAB is added, continue to stir 1.5h, add a certain amount of NiCl, stir 1.5h, be then slowly added dropwise
25% TMAOH, regulation pH value is 7,80 DEG C of reaction temperature, 25h is stirred at room temperature, and is filtered, washing, 80 DEG C of dryings, ball milling
Into the powder of certain particle diameter.Prepared sample is CTAB-Ni3PO4Fire retardant.
EVA/PA6/CTAB-Ni3PO4The preparation of/IFR composite flame-proof materials
Using melt intercalated method, the temperature for controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, and screw speed is
12r/min.30 parts of PP-g-MA is mixed for 9 parts with PA6 (carbon forming agent) first, then again with CTAB-Ni3PO41 part of mixing is equal
It is even, with double screw extruder extruding pelletization, then with its with masterbatch EVA60 parts the extruding pelletization again between 200~225 DEG C；System
Obtain EVA/PA6/CTAB-Ni3PO4/ IFR composite flame-proof materials.
The present invention can not be exhaustive one by one, in order that those skilled in the art further understands the present invention, below mainly with La
Salt is contrasted and tested, and is not intended to limit the present invention to other interest fields.
Embodiment 4
CTAB-LaPO4The preparation of fire retardant
According to n (Al2O3):n(P2O5):n(CTAB):n(H2O):n(TMAOH):n(LaCl3)=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% H3PO4It is added in 1000ml there-necked flask,
1h is stirred, adds a certain amount of CTAB, continues to stir 1h, adds a certain amount of LaCl3, 1h is stirred, is then slowly added dropwise
25% TMAOH, regulation pH value is 7,70 DEG C of reaction temperature, 24h is stirred at room temperature, and is filtered, washing, 80 DEG C of dryings, ball milling
Into the powder of certain particle diameter.Prepared sample is CTAB-LaPO4Fire retardant.
PP/PA6/CTAB-LaPO4The preparation of/IFR composite flame-proof materials
Using melt intercalated method, the temperature for controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, and screw speed is
12r/min.8 parts of PP-g-MA is mixed for 6.5 parts with PA6 (carbon forming agent) first, then again with CTAB-LaPO42.5 parts mixed
Close it is uniform, with double screw extruder extruding pelletization, then with its with masterbatch PP83 parts the extruding pelletization again between 200~225 DEG C；
PP/PA6/CTAB-LaPO is made4/ IFR composite flame-proof materials.
Embodiment 5
CTAB-LaPO4The preparation of fire retardant
According to n (Al2O3):n(P2O5):n(CTAB):n(H2O):n(TMAOH):n(LaCl3)=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% H3PO4It is added in 1000ml there-necked flask, stirs
0.5h, a certain amount of CTAB is added, continue to stir 0.5h, add a certain amount of LaCl3, 0.5h is stirred, is then slowly added dropwise
25% TMAOH, regulation pH value is 7,50 DEG C of reaction temperature, 20h is stirred at room temperature, and is filtered, washing, 80 DEG C of dryings, ball milling
Into the powder of certain particle diameter.Prepared sample is CTAB-LaPO4Fire retardant.
PP/PA6/CTAB-LaPO4The preparation of/IFR composite flame-proof materials
Using melt intercalated method, the temperature for controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, and screw speed is
12r/min.10 parts of PP-g-MA is mixed for 5 parts with PA6 (carbon forming agent) first, then again with CTAB-LaPO45 parts of mixing are equal
It is even, with double screw extruder extruding pelletization, then with its with masterbatch PP 80 parts of extruding pelletizations again between 200~225 DEG C；System
Obtain PP/PA6/CTAB-LaPO4/ IFR composite flame-proof materials.
Embodiment 6
CTAB-LaPO4The preparation of fire retardant
According to n (Al2O3):n(P2O5):n(CTAB):n(H2O):n(TMAOH):n(LaCl3)=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% H3PO4It is added in 1000ml there-necked flask, stirs
1.5h, a certain amount of CTAB is added, continue to stir 1.5h, add a certain amount of LaCl3, 1.5h is stirred, is then slowly added dropwise
25% TMAOH, regulation pH value is 7,80 DEG C of reaction temperature, 25h is stirred at room temperature, and is filtered, washing, 80 DEG C of dryings, ball milling
Into the powder of certain particle diameter.Prepared sample is CTAB-LaPO4Fire retardant.
PP/PA6/CTAB-LaPO4The preparation of/IFR composite flame-proof materials
Using melt intercalated method, the temperature for controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, and screw speed is
12r/min.22.5 parts of PP-g-MA is mixed for 9 parts with PA6 (carbon forming agent) first, then again with CTAB-LaPO47.5 parts mixed
Close it is uniform, with double screw extruder extruding pelletization, then with its with masterbatch PP60 parts the extruding pelletization again between 200~225 DEG C；
PP/PA6/CTAB-LaPO is made4/ IFR composite flame-proof materials.
Embodiment 7
CTAB-LAPO4The preparation of fire retardant
According to n (Al2O3):n(P2O5):n(CTAB):n(H2O):n(TMAOH):n(LaCl3)=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% H3PO4It is added in 1000ml there-necked flask, stirs
1h, a certain amount of CTAB is added, continue to stir 1h, add a certain amount of LaCl3, 1h is stirred, is then slowly added dropwise 25%
TMAOH, regulation pH value is 7,60 DEG C of reaction temperature, 24h is stirred at room temperature, and is filtered, and washing, 80 DEG C of dryings, ball milling is into certain
The powder of particle diameter.Prepared sample is CTAB-LaPO4Fire retardant.
PP/PA6/CTAB-LaPO4The preparation of/IFR composite flame-proof materials
Using melt intercalated method, the temperature for controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, and screw speed is
12r/min.15 parts of PP-g-MA is mixed for 8 parts with PA6 (carbon forming agent) first, then again with CTAB-LaPO410 parts of mixing
Uniformly, with double screw extruder extruding pelletization, then with its with masterbatch PP 67 parts of extruding pelletizations again between 200~225 DEG C,
PP/PA6/CTAB-LaPO is made4/ IFR composite flame-proof materials.
Fire retardant can also use to enter the methods of the precipitation method, sol-gel process, circumfluence method, solid reaction process in the present invention
It is prepared by row.
Above-described embodiment, simply presently preferred embodiments of the present invention, is not used for limiting the scope of the present invention, therefore all with this
The equivalent change or modification that feature and principle described in invention claim are done, all should be included in scope of the invention as claimed
Within.
Gained composite flame-proof material in obtained specific embodiment 4-7 is kneaded with double Kun kneading machines, then is ground into
Granular composite flame-proof material, mark batten finally is made with injection moulding machine and is used to test its fire resistance, and plastics its
His performance.
The experimental design formula of table 1
As can be seen from the above table：Work as CTAB-LaPO4When content is 5~6%, its intercalation-extent of exfoliation highest, point
Scattered property is best, and 10% and 42.2% is respectively increased in tensile strength and impact strength, and surplus charcoal rate reaches 7.78~10.12%, LOI and reached
To 22%, combustion testing reaches the HB levels of UL94 standards.In a word, CTAB-LaPO4Addition improve fire resistance and mechanics
Performance.
Claims (9)
1. a kind of composite flame-proof material, it is characterised in that be made by the following raw material calculated in parts by mass：
Wherein, the composite flame-proof material is prepared using melt intercalated method, the fire retardant is that CTAB- phosphate is fire-retardant
Agent, the CTAB- phosphate flame retardants are made by the following raw material of the amount proportioning by material：
Wherein, the CTAB- phosphate flame retardants are stratiform or mesoporous shape, and CTAB is cetyl trimethylammonium bromide, described
Weight/mass percentage composition of the CTAB- phosphate flame retardants in the composite flame-proof material is 5~6%.
2. composite flame-proof material as claimed in claim 1, it is characterised in that the inorganic salts be Fe, Zn, Ti, Mn, Mo, Cu,
Ni, Zr, Y, Ce, La nano phosphate.
3. composite flame-proof material as claimed in claim 1, it is characterised in that the phosphate is that percent by volume is 80%
Nano phosphate.
4. composite flame-proof material as claimed in claim 1, it is characterised in that the CTAB is ten that percent by volume is 25%
Six alkyl trimethyl ammonium bromides.
5. composite flame-proof material as claimed in claim 1, it is characterised in that the preparation side of the CTAB- phosphate flame retardants
Method is as follows：
A is mixed：
First the aluminum oxide of the amount and phosphoric acid are added in reactor, stirred 0.5~1.5 hour, then adds cetyl front three
Base ammonium bromide, continue stirring 0.5~1.5 hour, be subsequently added into halogen, stir 0.5~1.5 hour, tetrem is then slowly added dropwise
Base ammonium hydroxide, regulation pH value is 7, obtains mixture；
B reacts：
The reactor that the mixture is filled in step A is heated to 50~80 DEG C, stirring reaction 20~25 hours, is made
Reaction product；
C is post-processed：
Gained reaction product in step B is filtered, washed, dried, ball milling, the CTAB- phosphate flame retardants are made.
6. composite flame-proof material as claimed in claim 5, it is characterised in that the halogen be Fe, Zn, Ti, Mn, Mo, Cu,
Ni, Zr, Y, Ce, La hydrochloride.
7. composite flame-proof material as claimed in claim 1, it is characterised in that the masterbatch is in PE, PP, PS, PVC, ABS, EVA
One or more combination thing.
8. composite flame-proof material as claimed in claim 1, it is characterised in that the mass ratio of the PP-g-MA and PA6 are 3: 2.
9. prepare the method for composite flame-proof material described in any one in claim 7-8, it is characterised in that be specially：
The temperature for controlling dual-screw-stem machine is respectively 220 DEG C, 210 DEG C, 225 DEG C, screw speed 12r/min；First by PP-g-MA
Mixed with PA6 with the amount ratio, be then well mixed again with CTAB- phosphate flame retardants by the amount ratio, use twin-screw extrusion
Machine extruding pelletization, micelle is made；Finally by obtained micelle and masterbatch between 200~225 DEG C extruding pelletization again, be made
The composite flame-proof material containing CTAB- phosphate flame retardants.
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