CN104744820A - Polypropylene layered silicate nanometer composite material and preparation method thereof - Google Patents

Polypropylene layered silicate nanometer composite material and preparation method thereof Download PDF

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Publication number
CN104744820A
CN104744820A CN201510132907.8A CN201510132907A CN104744820A CN 104744820 A CN104744820 A CN 104744820A CN 201510132907 A CN201510132907 A CN 201510132907A CN 104744820 A CN104744820 A CN 104744820A
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polypropylene
composite material
modified
preparation
silicate
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李俊
代士维
段小刚
付伟
岳鲁敏
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Shanghai Institute of Technology
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Shanghai Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10Homopolymers or copolymers of propene
    • C08L23/12Polypropene
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/92Measuring, controlling or regulating
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F255/00Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
    • C08F255/02Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F285/00Macromolecular compounds obtained by polymerising monomers on to preformed graft polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
    • C08J3/22Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92504Controlled parameter
    • B29C2948/9258Velocity
    • B29C2948/9259Angular velocity
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92504Controlled parameter
    • B29C2948/92704Temperature
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/10Homopolymers or copolymers of propene
    • C08J2323/12Polypropene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2451/00Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

Abstract

The invention discloses a polypropylene layered silicate nanometer composite material and a preparation method thereof. The preparation method comprises the following steps of firstly performing intercalation modification on nanometer layered vermiculite by adopting modifier cetyl trimethyl ammonium bromide, thereby obtaining organic modified silicate; and then mixing obtained organic modified silicate with polypropylene which is modified by maleic anhydride with a grafting rate of 1 percent, adding styrene and butyl methacrylate into the mixture, dipping the mixture at a temperature of 30 DEG C for 1 h, and then rising the temperature of the mixture to 120 DEG C to perform reaction for 2h, drying the reactant under a vacuum condition to obtain modified masterbatch; calculating the masterbatch and polypropylene according to a mass ratio of masterbatch to polypropylene of 0.01 to 0.09: 1, pelleting after the polypropylene is mixed evenly on a high-speed mixing mill, and then controlling the temperature of 60 DEG C and drying the mixture for 12h to obtain the polypropylene layered silicate nanometer composite material. Compared with pure polypropylene, the polypropylene layered silicate nanometer composite material provided by the invention improves the mechanical property prominently.

Description

A kind of polypropylene laminated nm-silicate composite material and preparation method
Technical field
The present invention relates to a kind of polypropylene laminated nm-silicate composite material and preparation method, belong to technical field of material.
background field
Current by material modification, the correlated performance of material is significantly improved, and is the method that current Material Field is comparatively popular, wherein to polyolefin modified be the most promising.We know that polypropylene is as the universal material of engineering, because its molding shrinkage is large, low temperature brittleness, hardness are low, the easy shortcoming such as aging, poor heat resistance, limit polyacrylic application development, therefore study polypropylene/laminated nm-silicate composite material, have great importance.But polypropylene inherently nonpolar, polyolefine macromolecular material that surface energy is very low, layered silicate polarity is very strong, such polypropylene and layered silicate consistency very poor, therefore utilize fusion intercalation technology quite difficult.
The molecular weight of polypropylene itself is very large, and viscosity is large, and polypropylene macromolecular chain is difficult to enter in silicate layer.Current, solution carries out organic-treating to nano lamellar vermiculite, utilizes vermiculite interstitial inorganic cations and exchange with organic cation, makes nanometer vermiculite carry out organic-treating, reduce the polarity of nanometer vermiculite, make hydrophilic vermiculite surface-hydrophobicized.
Organising to nanometer vermiculite is a very complicated process, and it comprises particle dispersion, filters, washing, drying and other steps just can complete, higher to nanometer vermiculite modification cost, causes polyethylene/vermiculite nano composite material preparation cost significantly to increase.The polarity of nanometer vermiculite of organising just is reduced, and when carrying out melt blending, the consistency of material is improved, but to improve effect be not obvious especially.
Summary of the invention
An object of the present invention is to solve above-mentioned polypropylene and inorganic nano composite material poor compatibility and improving the technical problems such as polyacrylic mechanical property and provide a kind of preparation method of polypropylene laminated nm-silicate composite material.First this preparation method carries out organic-treating to nanometer vermiculite, obtain organic modified silicate and be mutually mixed with modified master with maleic anhydride modified polypropylene again, then by modified master, polypropylene mixing, granulation, drying, both obtained polypropylene laminated nm-silicate composite material.This preparation method overcome organic modification montmonrillonite directly with the shortcoming of polypropene blended poor performance, improve the performance of the polypropylene laminated nm-silicate composite material of final gained.
Two of object of the present invention is to provide the polypropylene laminated nm-silicate composite material of above-mentioned preparation method's gained.
Technical scheme of the present invention
A preparation method for polypropylene laminated nm-silicate composite material, specifically comprises the steps:
(1), nano lamellar vermiculite is first added in the reactor; then add distilled water to be uniformly mixed; pH is adjusted to be 7-8 with hydrochloric acid; properties-correcting agent cetyl trimethylammonium bromide is added after stirring 60min; at room temperature react 6h and intercalation modifying is carried out to nano lamellar vermiculite; in a nitrogen atmosphere, control temperature is 50-60 DEG C and carries out drying the reaction solution of gained, obtains organic modified silicate;
The consumption of above-mentioned nano lamellar vermiculite, distilled water, properties-correcting agent cetyl trimethylammonium bromide, calculates in mass ratio, i.e. nano lamellar vermiculite: distilled water: properties-correcting agent cetyl trimethylammonium bromide is that the ratio of 10g:12ml:1g calculates;
(2) the maleic anhydride modified polypropylene being, 1% by the organic modified silicate of step (1) gained and percentage of grafting mixes, then vinylbenzene, butyl methacrylate is added successively, control temperature is soak 1h at 30 DEG C, then 120 DEG C of stirring reaction 2h are warmed up to, discharging, products therefrom is vacuum-drying 2h at 60 DEG C, obtains modified master;
Above-mentioned organic modified silicate used, percentage of grafting are the amount of maleic anhydride modified polypropylene, vinylbenzene and the butyl methacrylate of 1%, calculate in mass ratio, i.e. organic modified silicate: percentage of grafting is the maleic anhydride modified polypropylene of 1%: vinylbenzene: butyl methacrylate is that the ratio of 10:10:7:1 is carried out;
Described percentage of grafting be 1% maleic anhydride modified polypropylene be prepared by a method comprising the following steps and form:
Thermometer is being housed, electric mixer, distilled water is added in the three-necked flask of the 500ml of reflux condensing tube, after being heated to 80 DEG C, add ammonium persulphate, MAH and PP powder carries out reaction 6h, the reacting liquid filtering of gained, it is neutral that the filter cake distilled water of gained carries out the pH washed to effluent liquid, then under vacuum with acetone extraction at least 6h, obtain the maleic anhydride modified polypropylene that percentage of grafting is 1%;
The consumption of above-mentioned distilled water, ammonium persulphate, MAH, PP powder, calculates, i.e. distilled water: ammonium persulphate in mass ratio: MAH:PP powder is 300:20:5:50.
(3), calculate in mass ratio, modified master: polypropylene is 0.01-0.4:1, be preferably 0.01-0.09:1, be more preferably the ratio of 0.05:1, after the modified master of polypropylene and step (2) gained is mixed on high speed mixing smelting machine, granulation is carried out by twin screw extruder, screw rod one to five temperature control district temperature is set as 190 DEG C respectively, 205 DEG C, 215 DEG C, 217 DEG C, 220 DEG C, in granulation process, the melt temperature of twin screw extruder is set as 200 DEG C, screw speed is 25r/min, granulation terminates rear control temperature and is 60 DEG C and carries out dry 12h, both polypropylene laminated nm-silicate composite material was obtained.
Beneficial effect of the present invention
The preparation method of polypropylene laminated nm-silicate composite material of the present invention, the properties-correcting agent cetyl trimethylammonium bromide being carried out ion-exchange by easy and vermiculite carries out to inorganic nano material and nano lamellar vermiculite the polarity that modification reduces inorganic nano material; And then coordinate maleic anhydride to strengthen its polarity to polypropylene modification, at swelling agent vinylbenzene, under butyl methacrylate effect, prepare modified master; Finally make it mix with polypropylene, prepare nanometer composite polypropylene material; And traditional method just carries out modification to wherein a kind of material, compared with traditional method, the method strengthens inorganic nano silicate and polyacrylic consistency further, and then significantly improve the mechanical property of material, the yield strength of a kind of polypropylene laminated nm-silicate composite material of gained, tensile strength, flexural strength, elongation at break, shock strength can reach respectively 27.9MPa, 43.5 MPa, 63.7MPa, 400%, 23.1J/m 2.
Accompanying drawing explanation
fig. 1,the pure PP of virgin pp batten and polypropylene laminated nm-silicate composite material batten PP-1, the stress strain curve figure of PP-2, PP-3, PP-4, PP-5.
Embodiment
Following by specific embodiment further describing in detail the present invention by reference to the accompanying drawings, but detailed example of the present invention is not merely limited to this.
embodiment 1
A preparation method for polypropylene laminated nm-silicate composite material, specifically comprises the steps:
(1), 50g nano lamellar vermiculite is first added in the reactor; then 60ml distilled water is added; being uniformly mixed rear hydrochloric acid adjusts pH to be 7-8; 5g properties-correcting agent cetyl trimethylammonium bromide is added after stirring 60min; at room temperature react 6h and intercalation modifying is carried out to nano lamellar vermiculite; in a nitrogen atmosphere, control temperature is 50-60 DEG C and carries out drying the reaction solution of gained, obtains organic modified silicate;
The consumption of above-mentioned nano lamellar vermiculite, distilled water, properties-correcting agent cetyl trimethylammonium bromide, calculates in mass ratio, i.e. nano lamellar vermiculite: distilled water: properties-correcting agent cetyl trimethylammonium bromide is that the ratio of 10g:12ml:1g calculates;
(2) the maleic anhydride modified polypropylene being, 1% by the organic modified silicate of 100g step (1) gained and 100g percentage of grafting mixes, then 70g vinylbenzene is added, 10g butyl methacrylate, 1h is soaked at 30 DEG C, then 120 DEG C are warmed up to, abundant stirring reaction 2h, discharging, products therefrom is vacuum-drying 2h at 60 DEG C, obtains dry good modified master;
Above-mentioned organic modified silicate used, percentage of grafting are the amount of maleic anhydride modified polypropylene, vinylbenzene and the butyl methacrylate of 1%, calculate in mass ratio, i.e. organic modified silicate: percentage of grafting is the maleic anhydride modified polypropylene of 1%: vinylbenzene: butyl methacrylate is that the ratio of 10:10:7:1 is carried out;
Described percentage of grafting be 1% maleic anhydride modified polypropylene be prepared by a method comprising the following steps and form:
Thermometer is being housed, electric mixer, add 300ml distilled water in the Mitsui flask of the 500ml of reflux condensing tube, being heated to temperature is 80 DEG C, then adds 20g ammonium persulphate (APS), 5 g MAH, 50g PP powder carries out reaction 6h, the reacting liquid filtering of gained, and it is neutral that the filter cake distilled water of gained carries out the pH washed to effluent liquid, then under vacuum with acetone extraction at least 6h, obtain the maleic anhydride modified polypropylene that percentage of grafting is 1%;
(3), calculate in mass ratio, modified master: polypropylene is the ratio of 0.01:1, by the modified master of 100g polypropylene and 1g step (2) gained, after high speed mixing smelting machine mixes, granulation is carried out by twin screw extruder, screw rod one to five temperature control district temperature is set as 190 DEG C respectively, 205 DEG C, 215 DEG C, 217 DEG C, 220 DEG C, in granulation process, the melt temperature of twin screw extruder is set as 200 DEG C, screw speed is 25r/min, and granulation terminates rear control temperature and is 60 DEG C and carries out dry 12h, both polypropylene laminated nm-silicate composite material.
embodiment 2
A preparation method for polypropylene laminated nm-silicate composite material, specifically comprises the steps:
(1), with the step (1) in embodiment 1;
(2), with the step (2) in embodiment 1;
(3), calculate in mass ratio, modified master: polypropylene is the ratio of 0.03:1, by the modified master of 100g polypropylene and 3g step (2) gained, after high speed mixing smelting machine mixes, granulation is carried out by twin screw extruder, screw rod one to five temperature control district temperature is set as 190 DEG C respectively, 205 DEG C, 215 DEG C, 217 DEG C, 220 DEG C, in granulation process, the melt temperature of twin screw extruder is set as 200 DEG C, screw speed is 25r/min, and granulation terminates rear control temperature and is 60 DEG C and carries out dry 12h, both polypropylene laminated nm-silicate composite material.
embodiment 3
A preparation method for polypropylene laminated nm-silicate composite material, specifically comprises the steps:
(1), with the step (1) in embodiment 1;
(2), with the step (2) in embodiment 1;
(3), calculate in mass ratio, modified master: polypropylene is the ratio of 0.05:1, by the modified master of 100g polypropylene and 5g step (2) gained, after high speed mixing smelting machine mixes, granulation is carried out by twin screw extruder, screw rod one to five temperature control district temperature is set as 190 DEG C respectively, 205 DEG C, 215 DEG C, 217 DEG C, 220 DEG C, in granulation process, the melt temperature of twin screw extruder is set as 200 DEG C, screw speed is 25r/min, and granulation terminates rear control temperature and is 60 DEG C and carries out dry 12h, both polypropylene laminated nm-silicate composite material.
embodiment 4
A preparation method for polypropylene laminated nm-silicate composite material, specifically comprises the steps:
(1), with the step (1) in embodiment 1;
(2), with the step (2) in embodiment 1;
(3), calculate in mass ratio, modified master: polypropylene is the ratio of 0.07:1, by the modified master of 100g polypropylene and 7g step (2) gained, after high speed mixing smelting machine mixes, granulation is carried out by twin screw extruder, screw rod one to five temperature control district temperature is set as 190 DEG C respectively, 205 DEG C, 215 DEG C, 217 DEG C, 220 DEG C, in granulation process, the melt temperature of twin screw extruder is set as 200 DEG C, screw speed is 25r/min, and granulation terminates rear control temperature and is 60 DEG C and carries out dry 12h, both polypropylene laminated nm-silicate composite material.
embodiment 5
A preparation method for polypropylene laminated nm-silicate composite material, specifically comprises the steps:
(1), with the step (1) in embodiment 1;
(2), with the step (2) in embodiment 1;
(3), calculate in mass ratio, modified master: polypropylene is the ratio of 0.09:1, by the modified master of 100g polypropylene and 9g step (2) gained, after high speed mixing smelting machine mixes, granulation is carried out by twin screw extruder, screw rod one to five temperature control district temperature is set as 190 DEG C respectively, 205 DEG C, 215 DEG C, 217 DEG C, 220 DEG C, in granulation process, the melt temperature of twin screw extruder is set as 200 DEG C, screw speed is 25r/min, and granulation terminates rear control temperature and is 60 DEG C and carries out dry 12h, both polypropylene laminated nm-silicate composite material.
By the polypropylene laminated nm-silicate composite material of virgin pp and above-described embodiment 1-5 gained respectively by hydropress, the each design temperature of upper and lower plates of hydropress is 210 DEG C, be pressed into virgin pp batten and polypropylene laminated nm-silicate composite material batten that length is respectively 20cm, 20cm, 4mm, be designated as pure PP, PP-1 respectively, PP-2, PP-3, PP-4, PP-5.
To the pure PP of virgin pp batten and the polypropylene laminated nm-silicate composite material batten PP-1 of above-mentioned gained, PP-2, PP-3, PP-4, PP-5 carry out Mechanics Performance Testing, and test result is as shown in the table:
Can draw from upper table, polypropylene laminated nm-silicate composite material batten PP-3, namely when modified master: when polypropylene is 0.05:1 (mass ratio), the yield strength of the polypropylene laminated nm-silicate composite material of gained, tensile strength, flexural strength, elongation at break, shock strength be respectively 27.9MPa, 43.5MPa, 63.7MPa, 400%, 23.1 J/m 2, the mechanical property of material reaches maximum value comparatively speaking, and comparatively virgin pp property indices is all significantly improved.
Adopt the BJDL-S type tension testing machine of Jinan platinum technical testing company limited to the pure PP of virgin pp batten of above-mentioned gained and polypropylene laminated nm-silicate composite material batten PP-1, PP-2, PP-3, PP-4, PP-5 carries out tensile property test, the stress strain curve of gained is shown in Fig. 1, as can be seen from Figure 1 the relevant mechanical property of material, and what indicate inorganic materials thus further adds the mechanical property can improving material.
In sum, a kind of polypropylene laminated nm-silicate composite material of preparation method's gained of the present invention, the consistency of Reinforced Polypropylene and nano inorganic material, compared with virgin pp, its mechanical property be improved significantly, its tensile strength can reach 38.2-43.5MPa, flexural strength 51.2-63.7MPa, yield strength 26.4-28.9MPa, elongation at break 201-455%, shock strength 18.7-23.1J/m 2.Particularly in preparation process when modified master: when polypropylene is 0.05:1 (mass ratio), the yield strength of a kind of polypropylene laminated nm-silicate composite material of gained, tensile strength, flexural strength, elongation at break, shock strength be respectively 27.9MPa, 43.5 MPa, 63.7MPa, 400%, 23.1J/m 2, namely mechanical property reaches maximum value comparatively speaking, and comparatively virgin pp property indices is all significantly improved.
The above is only the citing of embodiments of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.

Claims (8)

1. a preparation method for polypropylene laminated nm-silicate composite material, is characterized in that specifically comprising the steps:
(1), nano lamellar vermiculite is first added in the reactor; then add distilled water to be uniformly mixed; pH is adjusted to be 7-8 with hydrochloric acid; properties-correcting agent cetyl trimethylammonium bromide is added after stirring 60min; at room temperature react 6h and intercalation modifying is carried out to nano lamellar vermiculite; in a nitrogen atmosphere, control temperature is 50-60 DEG C and carries out drying the reaction solution of gained, obtains organic modified silicate;
The consumption of above-mentioned nano lamellar vermiculite, distilled water, properties-correcting agent cetyl trimethylammonium bromide, calculates in mass ratio, i.e. nano lamellar vermiculite: distilled water: properties-correcting agent cetyl trimethylammonium bromide is that the ratio of 10g:12ml:1g calculates;
(2) the maleic anhydride modified polypropylene being, 1% by the organic modified silicate of step (1) gained and percentage of grafting mixes, then vinylbenzene, butyl methacrylate is added successively, control temperature is soak 1h at 30 DEG C, then 120 DEG C of stirring reaction 2h are warmed up to, discharging, products therefrom is vacuum-drying 2h at 60 DEG C, obtains modified master;
Above-mentioned organic modified silicate used, percentage of grafting are the amount of maleic anhydride modified polypropylene, vinylbenzene and the butyl methacrylate of 1%, calculate in mass ratio, i.e. organic modified silicate: percentage of grafting is the maleic anhydride modified polypropylene of 1%: vinylbenzene: butyl methacrylate is that the ratio of 10:10:7:1 is carried out;
Described percentage of grafting be 1% maleic anhydride modified polypropylene be prepared by a method comprising the following steps and form:
Thermometer is being housed, electric mixer, distilled water is added in the three-necked flask of the 500ml of reflux condensing tube, after being heated to 80 DEG C, add ammonium persulphate, MAH and PP powder carries out reaction 6h, the reacting liquid filtering of gained, it is neutral that the filter cake distilled water of gained carries out the pH washed to effluent liquid, then under vacuum with acetone extraction at least 6h, obtain the maleic anhydride modified polypropylene that percentage of grafting is 1%;
The consumption of above-mentioned distilled water, ammonium persulphate, MAH, PP powder, calculates, i.e. distilled water: ammonium persulphate in mass ratio: MAH:PP powder is than being 300:20:5:50;
(3), calculate in mass ratio, modified master: polypropylene is the ratio of 0.01-0.4:1, after the modified master of polypropylene and step (2) gained is mixed on high speed mixing smelting machine, granulation is carried out by twin screw extruder, screw rod one to five temperature control district temperature is set as 190 DEG C respectively, 205 DEG C, 215 DEG C, 217 DEG C, 220 DEG C, in granulation process, the melt temperature of twin screw extruder is set as 200 DEG C, and screw speed is 25r/min, granulation terminates rear control temperature and is 60 DEG C and carries out dry 12h, both polypropylene laminated nm-silicate composite material.
2. the preparation method of a kind of polypropylene laminated nm-silicate composite material as claimed in claim 1, is characterized in that calculating in mass ratio in step (3), modified master: polypropylene is 0.01-0.09:1.
3. the preparation method of a kind of polypropylene laminated nm-silicate composite material as claimed in claim 1, is characterized in that calculating in mass ratio in step (3), modified master: polypropylene is 0.01-0.07:1.
4. the preparation method of a kind of polypropylene laminated nm-silicate composite material as claimed in claim 1, is characterized in that calculating in mass ratio in step (3), modified master: polypropylene is 0.01-0.05:1.
5. the preparation method of a kind of polypropylene laminated nm-silicate composite material as claimed in claim 1, is characterized in that calculating in mass ratio in step (3), modified master: polypropylene is 0.05-0.07:1.
6. the preparation method of a kind of polypropylene laminated nm-silicate composite material as claimed in claim 1, is characterized in that calculating in mass ratio in step (3), modified master: polypropylene is 0.05-0.09:1.
7. the preparation method of a kind of polypropylene laminated nm-silicate composite material as claimed in claim 1, is characterized in that calculating in mass ratio in step (3), modified master: polypropylene is 0.05:1.
8. the polypropylene laminated nm-silicate composite material of preparation method's gained as described in as arbitrary in claim 1-7.
CN201510132907.8A 2015-03-25 2015-03-25 Polypropylene layered silicate nanometer composite material and preparation method thereof Pending CN104744820A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
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CN106883511A (en) * 2017-02-23 2017-06-23 苏州纳贝通环境科技有限公司 A kind of low temperature resistant PP flexible pipes and preparation method thereof

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