CN1291625A - Nm-class unsaturated polyester/montmorillonite composition and its preparing process - Google Patents
Nm-class unsaturated polyester/montmorillonite composition and its preparing process Download PDFInfo
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- CN1291625A CN1291625A CN 00131572 CN00131572A CN1291625A CN 1291625 A CN1291625 A CN 1291625A CN 00131572 CN00131572 CN 00131572 CN 00131572 A CN00131572 A CN 00131572A CN 1291625 A CN1291625 A CN 1291625A
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Abstract
An nm-class unsaturated polyester/montmorillonite composition is prepared from prepolymer of unsaturated polyester resin (100 Wt. portions), organic montmorillonite processed by intercalation expanding (0.5-20), trigger (0.5-5.0) and promoter (0.5-5.0) through copolymerization to disintegrate the montmorillonite into nm particles which are uniformly dispersed in polyester matrix. Said composition has the improved mechanical and refractory performance.
Description
The invention belongs to a kind of unsaturated polyester (UP) matrix material and preparation method thereof, particularly a kind of nm-class unsaturated polyester/montmorillonite composition and preparation method thereof.
Unsaturated polyester (UP) is a kind of thermosetting material, is to use the most general thermosetting resin, this resin to add initiator generation Raolical polymerizable in the strongthener field, becomes insoluble infusible thermosetting material after the curing.At " Jongdoo Lee, Emmanuel p.Giannelis, Synthesis and Characterization of UnsaturatedPolyester and Phenolic Resin Nanoncomposites, Polymer Preprints, " reported in the document and a kind ofly mixed the nano composite material that obtains with unsaturated polyester with layered silicate, its thermostability is than the increasing of the virgin resin (thermal weight loss of the material of measuring and monitoring the growth of standing timber under 400 ℃ of temperature, the surplus heavy of matrix material is about 43%, the surplus heavy of virgin resin is about 35%), the Young's modulus of matrix material is than also the increasing of virgin resin (3Gpa → 4.5Gpa), but mechanical property and the resistance toheat of improving matrix material were not reported.
At " M.S.ISMAIL, M.A.M.ALI, A.A.EL-MILLIGY, M.S.AFIFI, Studies on Sand/ClayUnsaturated Polyester Composite Materials, Journal of Appied PolymerScience, 1999,72: 1031-1038 " reported a kind of matrix material that obtains with the mixture filling unsaturated polyester of sandy soil and clay in the document, wherein the weighting material size has bigger influence to performance of composites, when weighting material particle diameter during greater than 0.5mm, the ultimate compression strength of matrix material descends to some extent with the increase of weighting material content, and when weighting material particle diameter during less than 0.5mm, the ultimate compression strength of matrix material increases with the increase of weighting material content.Also compared the voidage and the water-absorbent of matrix material and virgin resin in the document, and analyzed the influence of weighting material particle diameter, the result shows that the weighting material particle diameter all increases greater than matrix material voidage and the water-absorbent of 0.5mm.But mechanical property and the resistance toheat of improving matrix material were not reported yet.
At " X.KORNMANN, L.A.BERGLUND, and J.STERTE, and E.P.GIANNELIS, Nanocomposites Based on Montmorillonite and Unsaturated Polyester, POLYMERENGINEERING AND SCIENCE, 1998,38 (8): 1351-1358; " reported that a kind of class montmorillonite filled unsaturated polyester of handling with silane coupling agent prepares the UP/CLAY nano composite material in the document, when polynite content was 1.5vol% in the matrix material, the energy-to-break of material (Gg) doubled (70J/m than virgin resin
2→ 138J/m
2), the Young's modulus of matrix material increases with the increase of polynite content, but mechanical property and the resistance toheat of improving matrix material were not reported yet.
The objective of the invention is to overcome weak point of the prior art, particularly having the unsaturated polyester of producing under the processing condition now, its mechanical property and resistance toheat can not satisfy the shortcoming of higher requirement.And provide a kind of nm-class unsaturated polyester/montmorillonite composition and preparation method thereof.This matrix material and preparation method thereof can improve the mechanical property and the resistance toheat of polymeric matrix under existing processing condition.
Technical solution of the present invention is as follows:
Polynite disperse phase yardstick is 10～100nm in the nm-class unsaturated polyester/montmorillonite composition of the present invention, its component and content following (weight part):
Unsaturated polyester resin performed polymer 100
Intercalation soil 0.5～20
Initiator 0.5～5.0
Promotor 0.5～5.0
Intercalation soil in the nm-class unsaturated polyester/montmorillonite composition component of the present invention is the organo montmorillonite through the processing of intercalation expansionization, and intercalation soil sheet interlayer spacing is 15～25_, its component and content following (weight part):
Polynite 0.5～20
Intercalator 0.12～8.00
Protonating agent 0.02～1.80
Unsaturated polyester resin performed polymer in the nm-class unsaturated polyester/montmorillonite composition component of the present invention is UP-196.It is with MALEIC ANHYDRIDE, Tetra hydro Phthalic anhydride, 1,2-propylene glycol and glycol ether and vinylbenzene be raw material prepared 196
#Unsaturated polyester.
Initiator in the nm-class unsaturated polyester/montmorillonite composition component of the present invention is cyclohexanone peroxide, benzoyl peroxide, methylethyl ketone peroxide.
Promotor in the nm-class unsaturated polyester/montmorillonite composition component of the present invention is cobalt naphthenate, xylidine, Diethyl Aniline.
Polynite raw material particle size during intercalation of the present invention local soil type divides is 30～80 μ m, and the cationic exchange total volume is 40～200mmol/100g, and montmorillonite layer thickness is 10_, and the cheating engaging layer spacing is 2～5_.
Intercalator during intercalation of the present invention local soil type divides is cetylamine, stearylamine, cetyl trimethylammonium bromide, acrylamide or its mixture.
Protonating agent during intercalation of the present invention local soil type divides is a protonic acid, as sulfuric acid, phosphoric acid, sulfonic acid, hydrochloric acid, acetic acid.
The method steps of nm-class unsaturated polyester/montmorillonite composition preparation of the present invention is as follows:
(1) preparation intercalation soil (polynite organically-modified):
The dispersion medium high speed of polynite at 10～1000 parts stirs in a, elder generation, forms stable suspensoid, and temperature of reaction is controlled at 50～90 ℃;
B, intercalator and protonating agent are added in the above-mentioned suspensoid, stir again and make it fully expanded, keep 4-24h, form suspension;
C, above-mentioned suspension is separated with supercentrifuge, then for several times with ethanol-water solution washing solid phase, to AgNO with 0.1M
3Do not contain CL in the solution check washing lotion
-Till;
Make intercalation soil after d, the vacuum-drying, its grinding and sieving is standby;
(2) preparation nm-class unsaturated polyester/montmorillonite composition
A, the unsaturated polyester performed polymer is joined in the polymerization reactor, add intercalation soil while stirring, stirred under the room temperature 1～5 hour;
B, drip initiator and promotor then in reactor, with above-mentioned system thorough mixing, closed system is evacuated to more than the vacuum tightness 0.09MPa under the room temperature while stirring, removes the bubble in the system, stops after 5～20 minutes stirring and stopping to vacuumize;
C, reactant is poured into mould, solidified under the room temperature 2～5 hours, under 80 ℃～100 ℃ temperature, solidified 2～3 hours again; Or reactant poured into mould, solidified 10 days under the room temperature; Can make nm-class unsaturated polyester/montmorillonite composition.
Nm-class unsaturated polyester/montmorillonite composition of the present invention prepares by in-situ inserted radical polymerization.In-situ inserted radical polymerization refers to polynite and makes intercalation soil through behind the intercalation of intercalator earlier, then it is carried out copolymerization as the 3rd monomer and unsaturated polyester performed polymer, intercalation soil (polynite after the processing) is dissociated into the nanometer lamella and is dispersed in the unsaturated polyester matrix in reaction, obtain nm-class unsaturated polyester/montmorillonite composition.Wherein used unsaturated polyester is a kind of resin prepolymer, and it is after being raw material reaction with MALEIC ANHYDRIDE, Tetra hydro Phthalic anhydride, 1,2-propylene glycol and glycol ether, and to going into the resin prepolymer of vinylbenzene preparation, its structural formula is as follows:
Polynite during intercalation local soil type divides is class mineral, and major ingredient is for containing the layered silicate of 80%-95% polynite (Mont).Polynite is multiple layer mineral, its unit cell be by add in the middle of two drift angles Si-O tetrahedron inwardly a slice Al (O, OH) the octahedra composition rely on shared Sauerstoffatom to be connected between tetrahedron and the octahedron, continuous between the structure cell for the oxygen layer.The lamellar spacing of polynite is 1.0nm.The lamella internal surface has negative charge, and its specific surface area is 200～800m
2/ g, interlayer cation are Na
+, Ca
2+, Mg
2+, or Al
3+Deng genus interchangeability positively charged ion.After adopting organic amine (ammonium) salt quasi-molecule and montmorillonite polynite to carry out ion exchange reaction, the polynite interfloor distance is widened, be easy to the sheet interlayer that the unsaturated polyester performed polymer is inserted into polynite.Selected polynite thereby the cationic exchange total volume (CEC) that should have are 40～200mmol/100g.The polynite raw material particle size is at 30～80 μ m, and montmorillonite layer thickness is 10_, and the cheating engaging layer spacing is 2～5_.Intercalation soil sheet interlayer spacing behind intercalation polymeric is increased to 25～50_, and the montmorillonite layer spacing is bigger, and performance of composites better.
Polynite content is 0.5～20 (weight part) in the present invention, and when content is lower than 0.5 part, polynite is not enough to produce enough enhancements and thermotolerance; When content surpasses 20 parts, the mechanical property of matrix material descends on the contrary, and the transparency of matrix material also obviously descends simultaneously.
Behind above-mentioned performed polymer and polynite (intercalation soil) uniform mixing after intercalator is handled, add suitable initiator and promotor, Raolical polymerizable can take place and obtain insoluble infusible thermosetting resin in system.
The present invention compared with prior art has following advantage:
1, in-situ inserted polymerization technique provided by the invention is at first intercalator to be inserted into accurate two-dimentional silicate montmorillonite material lamella chien shih montmorillonite layer to strut, and then rely on macromolecular chain macromolecular chain to be inserted into the silicate plate interlayer and lamella is dissociated with the interaction between the intercalator organic group, thereby polynite reaches the homodisperse of nanoscale, forms nano composite polymer-montmorillonoid material.Compare with changing processing condition, the present invention is simple to operate, is easy to suitability for industrialized production, and performance improves a lot.
2, the nm-class unsaturated polyester/montmorillonite composition of the present invention's preparation, be dispersed in polynite in the unsaturated polyester performed polymer with 10～100nm yardstick, has very large interfacial area, very strong interaction is arranged between inorganic phase and polymeric matrix, can give full play to the rigidity and the resistance toheat of inorganics, and the thermotolerance of gained matrix material and resistance to impact shock there is more obviously raising than virgin resin.Sample testing is the result show: the resistance to impact shock of matrix material has improved 2.2 times, and tensile strength improved 12%, has realized toughness reinforcing enhancing.The heat-drawn wire of matrix material has improved 8 ℃, and macroscopic view is reliable more than simple thermogravimetic analysis (TGA).
The invention will be further described below in conjunction with embodiment: embodiment 1:
(1) preparation intercalation soil (polynite organically-modified)
A, elder generation are the polynite 20g of 100mmol/100g with the cationic exchange total volume, and the dispersion medium ethanol water mixture high speed stirring at 500g forms stable suspensoid, and temperature of reaction is controlled at 70～75 ℃;
B, add intercalator cetylamine 4.82g and protonating agent concentrated hydrochloric acid 1.7g in above-mentioned suspensoid, stir and make it fully expanded, the reaction times is 16 hours;
After c, above-mentioned reaction finish, separate solid phase and water, with ethanol-water solution washing solid phase for several times, use the AgNO of 0.1M more then with supercentrifuge
3Do not contain CL in the solution check washing lotion
-Till;
Make intercalation soil after d, the vacuum-drying, its grinding and sieving is standby.(2) preparation nm-class unsaturated polyester/montmorillonite composition
A, the UP performed polymer of getting 100g join in the polymerization reactor, add intercalation soil (polynite after the processing) high-speed stirring 1 hour of 1.0g, make the two thorough mixing even;
B, in reactor, add 2.0g initiator cyclohexanone peroxide and 1.0g promotor cobalt naphthenate, with above-mentioned system thorough mixing, closed system, being evacuated to vacuum tightness under the room temperature while stirring is 0.09MPa, remove the bubble in the system, stop after 20 minutes stirring and vacuum;
C, reactant is poured into mould, solidified 2 hours under the room temperature, solidified 2 hours down at 80 ℃ again, can make unsaturated polyester/Nano composite material of montmorillonite.
The polynite disperse phase is dispersed in the unsaturated polyester matrix with 50～100nm yardstick after tested.The structure of gained matrix material and performance see Table 1, table 2.Embodiment 2:
(1) preparation intercalation soil (polynite organically-modified)
A, elder generation are the polynite 10g of 100mmol/100g with the cationic exchange total volume, and the dispersion medium ethanol water mixture high speed stirring at 500g forms stable suspensoid, and temperature of reaction is controlled at 70～75 ℃;
B, add intercalator cetylamine 1.2g and acrylamide 1.0g and protonating agent concentrated hydrochloric acid 1.50g in above-mentioned suspensoid, stir and make it fully expanded, the reaction times is 16 hours;
After c, above-mentioned reaction finish, separate solid phase and water, with ethanol-water solution washing solid phase for several times, use the AgNO of 0.1M more then with supercentrifuge
3Do not contain CL in the solution check washing lotion
-Till;
Make intercalation soil after d, the vacuum-drying, its grinding and sieving is standby.
(2) preparation nm-class unsaturated polyester/montmorillonite composition
A, the UP performed polymer of getting 100g add in the polymerization reactor, add intercalation soil (polynite after the processing) high-speed stirring 1 hour of 1.0g, make the two thorough mixing even;
B, in reactor, add 1.5g initiator cyclohexanone peroxide and 1.0g promotor cobalt naphthenate, with above-mentioned system thorough mixing, being evacuated to vacuum tightness under the closed system room temperature while stirring is 0.09MPa, removes the bubble in the system, stops after 7 minutes stirring and vacuum;
C, reactant is poured into mould, solidified 2 hours under the room temperature, solidified 2 hours down at 80 ℃ again, can make unsaturated polyester/Nano composite material of montmorillonite;
The polynite disperse phase is dispersed in the unsaturated polyester matrix with 10～100nm yardstick after tested.The structure of gained matrix material and performance see Table 1, table 2.Embodiment 3:
(1) preparation intercalation soil (polynite organically-modified)
A, elder generation are the montmorillonite polynite 20g of 100mmol/100g with the cationic exchange total volume, and the dispersion medium ethanol water mixture high speed stirring at 500g forms stable suspensoid, and temperature of reaction is controlled at 70～75 ℃;
B, add intercalator stearylamine 5.4g and protonating agent concentrated hydrochloric acid 1.5g in above-mentioned suspensoid, stir and make it fully expanded, the reaction times is 16 hours;
After c, above-mentioned reaction finish, separate solid phase and water, with ethanol-water solution washing solid phase for several times, use the AgNO of 0.1M more then with supercentrifuge
3Do not contain CL in the solution check washing lotion
-Till;
Make intercalation soil after d, the vacuum-drying, its grinding and sieving is standby.
(2) preparation nm-class unsaturated polyester/montmorillonite composition
A, the UP performed polymer of getting 100g add in the polymerization reactor, and the intercalation soil of 1.0g (polynite after the processing) high-speed stirring 1 hour makes the two thorough mixing even;
B, in reactor, add 2.0g initiator cyclohexanone peroxide and 1.5g promotor cobalt naphthenate, with above-mentioned system thorough mixing, being evacuated to vacuum tightness under the closed system room temperature while stirring is 0.09MPa, removes the bubble in the system, stops after 15 minutes stirring and vacuum;
C, reactant is poured into mould, solidified 2 hours under the room temperature, solidified 2 hours down at 80 ℃ again, can make unsaturated polyester/Nano composite material of montmorillonite.
The polynite disperse phase is dispersed in the unsaturated polyester matrix with 50～100nm yardstick after tested.The structure of gained matrix material and performance see Table 1, table 2.Embodiment 4:
(1) preparation intercalation soil (polynite organically-modified)
A, elder generation are the polynite 12g of 100mmol/100g with the cationic exchange total volume, and the dispersion medium ethanol water mixture high speed stirring at 500g forms stable suspensoid, and temperature of reaction is controlled at 70～75 ℃;
B, add intercalator acrylamide 1.4g and protonating agent concentrated hydrochloric acid 1.8g in above-mentioned suspensoid, stir and make it fully expanded, the reaction times is 16 hours;
After c, above-mentioned reaction finish, separate solid phase and water, with ethanol-water solution washing solid phase for several times, use the AgNO of 0.1M more then with supercentrifuge
3Do not contain CL in the solution check washing lotion
-Till;
Make intercalation soil after d, the vacuum-drying, its grinding and sieving is standby.
(2) preparation nm-class unsaturated polyester/montmorillonite composition
A, the UP performed polymer of getting 100g add in the polymerization reactor, add intercalation soil (polynite after the processing) high-speed stirring 1 hour of 1.0g, make the two thorough mixing even;
B, in reactor, add 0.5g initiator cyclohexanone peroxide and 1.0g promotor cobalt naphthenate, with above-mentioned system thorough mixing, being evacuated to vacuum tightness under the closed system room temperature while stirring is 0.09MPa, removes the bubble in the system, stops after 10 minutes stirring and vacuum;
C, reactant is poured into mould, solidified 2 hours under the room temperature, solidified 2 hours down at 80 ℃ again, can make unsaturated polyester/Nano composite material of montmorillonite.
The polynite disperse phase is dispersed in the unsaturated polyester matrix with 30～100nm yardstick after tested.The structure of gained matrix material and performance see Table 1, table 2.Embodiment 5:
(1) preparation intercalation soil (polynite organically-modified)
A, elder generation are the montmorillonite polynite 15g of 100mmol/100g with the cationic exchange total volume, and the dispersion medium ethanol water mixture high speed stirring at 500g forms stable suspensoid, and temperature of reaction is controlled at 70～75 ℃;
B, add intercalator cetyl trimethylammonium bromide 7.5g in above-mentioned suspensoid, stir and make it fully expanded, the reaction times is 16 hours;
After c, above-mentioned reaction finish, separate solid phase and water, with ethanol-water solution washing solid phase for several times, use the AgNO of 0.1M more then with supercentrifuge
3Do not contain CL in the solution check washing lotion
-Till;
Make intercalation soil after d, the vacuum-drying, its grinding and sieving is standby.
(2) preparation nm-class unsaturated polyester/montmorillonite composition
A, the UP performed polymer of getting 100g add in the polymerization reactor, add intercalation soil (polynite after the processing) high-speed stirring 1 hour of 1.0g, make the two thorough mixing even;
B, in reactor, add 4.0g initiator cyclohexanone peroxide and 0.5g promotor cobalt naphthenate, with above-mentioned system thorough mixing, being evacuated to vacuum tightness under the closed system room temperature while stirring is 0.09MPa, removes the bubble in the system, stops after 8 minutes stirring and vacuum;
C, reactant is poured into mould, solidified 2 hours under the room temperature, solidified 2 hours down at 80 ℃ again, can make unsaturated polyester/Nano composite material of montmorillonite.
The polynite disperse phase is dispersed in the unsaturated polyester matrix with 30～100nm yardstick after tested.The structure of gained matrix material and performance see Table 1, table 2.
Embodiment 6～9 preparation methods are identical with embodiment 2, and wherein the consumption of intercalation soil (polynite after the processing) is respectively 2g, 3g, 5g, 10g, and the consumption of initiator and promotor is also identical with embodiment 2.Its mechanical property sees Table 2.
Table 1: the Micro-Structure Analysis of nm-class unsaturated polyester/montmorillonite composition
| Embodiment | Intercalation soil consumption (g) | Estrodur performed polymer content (g) is closed in insatiable hunger | The spacing d of intercalation soil 001(nm) | The spacing d of matrix material 001(nm) | Polynite disperse phase yardstick (nm) |
| 1 | 1．0 | 100 | 2．551 | 2．830 | 50-100 |
| 2 | 1．0 | 100 | 1．738 | ＞6．79 | 10-100 |
| 3 | 1．0 | 100 | 1．863 | 2．075 | 50-100 |
| 4 | 1．0 | 100 | 1．544 | 1．825 | 30-100 |
| 5 | 1．0 | 100 | 2．291 | 2．378 | 30-100 |
The result of table 1 shows that the spacing of polynite improves a lot in the gained nm-class unsaturated polyester/montmorillonite composition, and the polynite disperse phase is dispersed in the UP matrix with median size 10～100nm.
Table 2: the mechanical property of nm-class unsaturated polyester/montmorillonite composition and resistance toheat
| Embodiment | Intercalation soil consumption (g) | Unsaturated polyester performed polymer content (g) | Unnotched impact strength (KJ/m 2) | Tensile strength (MPa) | Heat-drawn wire HDT (℃) |
| ????100 | ????2.594 | ????64.70 | ????76.3 | ||
| ????1 | ????1.0 | ????100 | ????5.703 | ????72.06 | ????81.6 |
| ????2 | ????1.0 | ????100 | ????4.295 | ????67.89 | ????78.4 |
| ????3 | ????1.0 | ????100 | ????5.079 | ????69.21 | ????78.9 |
| ????4 | ????1.0 | ????100 | ????4.867 | ????70.14 | ????80.2 |
| ????5 | ????1.0 | ????100 | ????5.351 | ????65.73 | ????79.6 |
| ????6 | ????2.0 | ????100 | ????8.009 | ????72.61 | ????84.5 |
| ????7 | ????3.0 | ????100 | ????8.484 | ????65.66 | ????80.7 |
| ????8 | ????5.0 | ????100 | ????2.810 | ????51.11 | ????79.2 |
| ????9 | ????10.0 | ????100 | ????2.746 | ????50.79 | ????85.3 |
The result of table 2 shows that the shock strength of gained nm-class unsaturated polyester/montmorillonite composition improves more than 2 times, and heat-drawn wire improves about 8 ℃, and tensile strength does not reduce.
Claims (10)
1, a kind of nm-class unsaturated polyester/montmorillonite composition is characterized in that: polynite disperse phase yardstick is 10-100nm in the matrix material, its component and content following (weight part):
Unsaturated polyester resin performed polymer 100
Intercalation soil 0.5～20
Initiator 0.5～5.0
Promotor 0.5～5.0
2, according to the said nm-class unsaturated polyester/montmorillonite composition of claim 1, it is characterized in that: the intercalation soil in the matrix material component is the organo montmorillonite through the processing of intercalation expansionization, intercalation soil sheet interlayer spacing is 15-25_, its component and content following (weight part):
Polynite 0.5～20
Intercalator 0.12～8.00
Protonating agent 0.02～1.80
3, according to the described nm-class unsaturated polyester/montmorillonite composition of claim 1, it is characterized in that: the unsaturated polyester resin performed polymer in the matrix material component is UP-196.
4, according to the described nm-class unsaturated polyester/montmorillonite composition of claim 1, it is characterized in that: the initiator in the matrix material component is cyclohexanone peroxide, benzoyl peroxide, methylethyl ketone peroxide.
5, according to the described nm-class unsaturated polyester/montmorillonite composition of claim 1, it is characterized in that: the promotor in the matrix material component is cobalt naphthenate, xylidine, Diethyl Aniline.
6, according to the said intercalation soil of claim 2, it is characterized in that: the polynite raw material particle size during described intercalation local soil type divides is 30～80 μ m, the cationic exchange total volume is 40～200mmol/100g, and montmorillonite layer thickness is 10_, and the cheating engaging layer spacing is 2～5_.
7, according to the described intercalation soil of claim 2, it is characterized in that: the intercalator during described intercalation local soil type divides is cetylamine, stearylamine, cetyl trimethylammonium bromide, acrylamide or its mixture.
8, according to the described intercalation soil of claim 2, it is characterized in that: the protonating agent during described intercalation local soil type divides is a protonic acid, as sulfuric acid, phosphoric acid, sulfonic acid, hydrochloric acid, acetic acid.
9, as the preparation method of claim 1 and 2 said nm-class unsaturated polyester/montmorillonite compositions, it is characterized in that: the method steps of Composite Preparation is as follows:
(1) preparation intercalation soil (polynite organically-modified):
The dispersion medium high speed of polynite at 10～1000 parts stirs in a, elder generation, forms stable suspensoid, and temperature of reaction is controlled at 50～90 ℃;
B, intercalator and protonating agent are added in the above-mentioned suspensoid, stir again and make it fully expanded, kept 4～24 hours, form suspension;
C, above-mentioned suspension is separated with supercentrifuge, then for several times with ethanol-water solution washing solid phase, to AgNO with 0.1M
3Do not contain CL in the solution check washing lotion
-Till;
Make intercalation soil after d, the vacuum-drying, its grinding and sieving is standby;
(2) preparation nm-class unsaturated polyester/montmorillonite composition
A, the unsaturated polyester performed polymer is joined in the polymerization reactor, add intercalation soil while stirring, stirred under the room temperature 1～5 hour;
B, in reactor, drip initiator and promotor then,, be evacuated to vacuum tightness under the room temperature while stirring, remove the bubble in the system, stop after 5～20 minutes stirring and stopping to vacuumize greater than 0.09MPa with above-mentioned system thorough mixing, closed system;
C, reactant is poured into mould, solidify 2～5 hours under the room temperature after, under 80 ℃～100 ℃ temperature, solidified 2～3 hours again, can make nm-class unsaturated polyester/montmorillonite composition.
10, according to the preparation method of the said nm-class unsaturated polyester/montmorillonite composition of claim 9, it is characterized in that: the solidification process of reactant can pour into mould with reactant in the preparation of matrix material, solidified 10 days under the room temperature, also can make nm-class unsaturated polyester/montmorillonite composition.
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2000
- 2000-10-28 CN CN 00131572 patent/CN1121450C/en not_active Expired - Fee Related
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| CN114773816B (en) * | 2022-05-24 | 2024-05-17 | 新阳科技集团有限公司 | Flame-retardant unsaturated polyester resin composite material and preparation method thereof |
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