CN102352138A - Organic modification method of montmorillonite flame retardant - Google Patents
Organic modification method of montmorillonite flame retardant Download PDFInfo
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- CN102352138A CN102352138A CN2011102353574A CN201110235357A CN102352138A CN 102352138 A CN102352138 A CN 102352138A CN 2011102353574 A CN2011102353574 A CN 2011102353574A CN 201110235357 A CN201110235357 A CN 201110235357A CN 102352138 A CN102352138 A CN 102352138A
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- polynite
- ball milling
- organic modification
- montmorillonite
- slurry
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- 229910052901 montmorillonite Inorganic materials 0.000 title claims abstract description 26
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 title claims abstract description 25
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title abstract description 3
- 239000003063 flame retardant Substances 0.000 title abstract description 3
- 238000002715 modification method Methods 0.000 title abstract 3
- 230000004048 modification Effects 0.000 claims abstract description 63
- 238000012986 modification Methods 0.000 claims abstract description 63
- 238000000498 ball milling Methods 0.000 claims abstract description 52
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000003607 modifier Substances 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims description 47
- 239000000203 mixture Substances 0.000 claims description 37
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical group [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 22
- 239000012757 flame retardant agent Substances 0.000 claims description 15
- 150000001768 cations Chemical class 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 150000001767 cationic compounds Chemical class 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 3
- 229910001411 inorganic cation Inorganic materials 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 3
- 150000002892 organic cations Chemical class 0.000 abstract description 3
- 239000012074 organic phase Substances 0.000 abstract description 3
- 125000002091 cationic group Chemical group 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 238000000197 pyrolysis Methods 0.000 abstract description 2
- 229910017059 organic montmorillonite Inorganic materials 0.000 abstract 1
- 238000004537 pulping Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- -1 organo montmorillonite Chemical compound 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 235000021321 essential mineral Nutrition 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Silicates, Zeolites, And Molecular Sieves (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
蒙脱土阻燃剂有机改性方法属于蒙脱土改性技术领域；所要解决的技术问题为提供了一种制备良好相容性且蒙脱土片层易于剥离的改性方法；所采用的技术方案为：第一步制浆，第二步调pH值，第三步加入阳离子改性剂，第四步球磨，第五步烘干，第六步再球磨得到成品有机改性蒙脱土；本发明采用球磨改性的方法，有效提高了与有机基体的相容性，以及降低了有机蒙脱土的热解速率，减小蒙脱土的粒径，蒙脱土层间的大量无机阳离子已被有机改性剂的有机阳离子所置换，其与有机相的相容性增大了3-6倍，并改变其分散状态，分散会更加均匀，并且操作过程简单，易于制备。The organic modification method of montmorillonite flame retardant belongs to the field of montmorillonite modification technology; the technical problem to be solved is to provide a modification method for preparing good compatibility and easy peeling of montmorillonite sheets; the adopted technology The scheme is: the first step is pulping, the second step is to adjust the pH value, the third step is to add cationic modifier, the fourth step is ball milling, the fifth step is drying, and the sixth step is ball milling to obtain the finished organic modified montmorillonite; The invention adopts the method of ball milling modification, which effectively improves the compatibility with the organic matrix, reduces the pyrolysis rate of the organic montmorillonite, reduces the particle size of the montmorillonite, and a large amount of inorganic cations between the layers of the montmorillonite have been eliminated. Replaced by the organic cation of the organic modifier, its compatibility with the organic phase is increased by 3-6 times, and its dispersion state is changed, the dispersion will be more uniform, and the operation process is simple and easy to prepare.
Description
Technical field
The organically-modified method of montmorillonite flame-retardant agent of the present invention belongs to imvite modified technical field.
Background technology
Polynite is the essential mineral composition of POLARGEL NF rock, is a kind of typical laminated clay, has the specific surface area (750m of super large
2/ g) with up to the footpath/thickness rate more than 200, can improve the mechanical property and the thermostability of polymer composites significantly as filler, reduce the rate of permeation of gas and steam, obtained application widely in flame retardant area.
A large amount of mineral ions show as hydrophilic oleophobic property because of interlayer has in polynite, be unfavorable for its in organic phase dispersion and to the absorption of organic substance.When polynite is applied to organic system, must carry out organically-modified to it; Promptly replace the inorganic cation in the polynite (referring generally to sodium-based montmorillonite) with organic cation; To change the cationic form and the interlayer ion form of polynite crystal layer, make it surface-hydrophobicized.And utilize chemical process organically-modified to polynite, its complete processing has very big influence to lamella, has destroyed the microstructure homogeneity of organo montmorillonite, makes its laminated structure degradation.
Summary of the invention
The present invention overcomes the deficiency of prior art, and technical problem to be solved is that a kind of imvite modified method that excellent compatibility and montmorillonite layer are easy to peel off for preparing is provided.
In order to solve the problems of the technologies described above, the technical scheme that the present invention adopts is for to carry out according to following steps:
The organically-modified method of montmorillonite flame-retardant agent, carry out according to following steps:
The first step, slurrying
The deionized water of polynite with 60 ℃-85 ℃ mixed, stir, obtain the polynite slurry, the weight part ratio of said polynite and deionized water is 1:0.5-2;
Second step, adjust pH
With the sodium hydroxide solution of weight percent concentration 3%-8%, regulate said polynite slurry pH value to 8-9, obtain alkaline polynite slurry;
In the 3rd step, add cation modifier
Is that 30-60:1 mix with cation modifier according to weight part ratio with said alkaline polynite slurry, stirs, and obtains imvite modified mixture;
The 4th step, ball milling
Said imvite modified mixture is put into ball mill, ball milling 4-8 hour, obtain organic modification montmonrillonite;
The 5th step, oven dry
Said organic modification montmonrillonite is put into oven for drying, and 70 ℃-80 ℃ of temperature time 15-25 hour, obtain the exsiccant organic modification montmonrillonite;
The 6th step, ball milling again
With said exsiccant organic modification montmonrillonite in ball mill ball milling 0.5-2 hour once more, sieve then, sieve aperture is the 200-400 order, obtains the finished product organic modification montmonrillonite.
Described cation modifier is an octadecyl trimethyl ammonium chloride.
The present invention compared with prior art has following beneficial effect.
The present invention adopts the method for ball milling modification; Effectively improved consistency with polymer matrix; And the pyrolysis rate that has reduced organo montmorillonite; Reduce the particle diameter of polynite, a large amount of inorganic cations between cheating engaging layer are replaced by the organic cation of organic modifiers, and the consistency of itself and organic phase has increased 3-6 doubly; Be prone to realize montmorillonite layer peeling off in polymer matrix; Divide breaking up more even, and operating process is simple, is easy to preparation.
Embodiment
Embodiment 1, and the organically-modified method of montmorillonite flame-retardant agent is carried out according to following steps:
The first step, slurrying
The deionized water of polynite with 60 ℃ mixed, stir, obtain the polynite slurry, the weight part ratio of said polynite and deionized water is 1:0.5;
Second step, adjust pH
With the sodium hydroxide solution of weight percent concentration 3%, regulate said polynite pH value to 8, obtain alkaline polynite slurry;
In the 3rd step, add octadecyl trimethyl ammonium chloride
Is that 30:1 mix with octadecyl trimethyl ammonium chloride according to weight part ratio with said alkaline polynite slurry, stirs, and obtains imvite modified mixture;
The 4th step, ball milling
Said imvite modified mixture is put into ball mill, and ball milling 4 hours obtains organic modification montmonrillonite;
The 5th step, oven dry
Said organic modification montmonrillonite is put into oven for drying, and 70 ℃ of temperature, obtain the exsiccant organic modification montmonrillonite at 15 hours time;
The 6th step, ball milling again
With said exsiccant organic modification montmonrillonite ball milling 2 hours once more in ball mill, sieve then, sieve aperture is 200 orders, obtains the finished product organic modification montmonrillonite.
Embodiment 2, and the organically-modified method of montmorillonite flame-retardant agent is carried out according to following steps:
The first step, slurrying
The deionized water of polynite with 85 ℃ mixed, stir, obtain the polynite slurry, the weight part ratio of said polynite and deionized water is 1:2;
Second step, adjust pH
With the sodium hydroxide solution of weight percent concentration 8%, regulate said polynite slurry pH value to 9, obtain alkaline polynite slurry;
In the 3rd step, add octadecyl trimethyl ammonium chloride
Is that 60:1 mix with octadecyl trimethyl ammonium chloride according to weight part ratio with said alkaline polynite slurry, stirs, and obtains imvite modified mixture;
The 4th step, ball milling
Said imvite modified mixture is put into ball mill, and ball milling 5 hours obtains organic modification montmonrillonite;
The 5th step, oven dry
Said organic modification montmonrillonite is put into oven for drying, and 80 ℃ of temperature, obtain the exsiccant organic modification montmonrillonite at 25 hours time;
The 6th step, ball milling again
With said exsiccant organic modification montmonrillonite ball milling 1.5 hours once more in ball mill, sieve then, sieve aperture is 230 orders, obtains the finished product organic modification montmonrillonite.
Embodiment 3, and the organically-modified method of montmorillonite flame-retardant agent is carried out according to following steps:
The first step, slurrying
The deionized water of polynite with 75 ℃ mixed, stir, obtain the polynite slurry, the weight part ratio of said polynite and deionized water is 1:1.5;
Second step, adjust pH
With the sodium hydroxide solution of weight percent concentration 5%, regulate said polynite slurry pH value to 8.5, obtain alkaline polynite slurry;
In the 3rd step, add octadecyl trimethyl ammonium chloride
Is that 45:1 mix with octadecyl trimethyl ammonium chloride according to weight part ratio with said alkaline polynite slurry, stirs, and obtains imvite modified mixture;
The 4th step, ball milling
Said imvite modified mixture is put into ball mill, and ball milling 6 hours obtains organic modification montmonrillonite;
The 5th step, oven dry
Said organic modification montmonrillonite is put into oven for drying, and 75 ℃ of temperature, obtain the exsiccant organic modification montmonrillonite at 20 hours time;
The 6th step, ball milling again
With said exsiccant organic modification montmonrillonite ball milling 1 hour once more in ball mill, sieve then, sieve aperture is 270 orders, obtains the finished product organic modification montmonrillonite.
Embodiment 4, and the organically-modified method of montmorillonite flame-retardant agent is carried out according to following steps:
The first step, slurrying
The deionized water of polynite with 65 ℃ mixed, stir, obtain the polynite slurry, the weight part ratio of said polynite and deionized water is 1:2;
Second step, adjust pH
With the sodium hydroxide solution of weight percent concentration 7%, regulate said polynite slurry pH value to 8, obtain alkaline polynite slurry;
In the 3rd step, add octadecyl trimethyl ammonium chloride
Is that 40:1 mix with octadecyl trimethyl ammonium chloride according to weight part ratio with said alkaline polynite slurry, stirs, and obtains imvite modified mixture;
The 4th step, ball milling
Said imvite modified mixture is put into ball mill, and ball milling 7 hours obtains organic modification montmonrillonite;
The 5th step, oven dry
Said organic modification montmonrillonite is put into oven for drying, and 73 ℃ of temperature, obtain the exsiccant organic modification montmonrillonite at 22 hours time;
The 6th step, ball milling again
With said exsiccant organic modification montmonrillonite ball milling 1 hour once more in ball mill, sieve then, sieve aperture is 325 orders, obtains the finished product organic modification montmonrillonite.
Embodiment 5, and the organically-modified method of montmorillonite flame-retardant agent is carried out according to following steps:
The first step, slurrying
The deionized water of polynite with 80 ℃ mixed, stir, obtain the polynite slurry, the weight part ratio of said polynite and deionized water is 1:1.5;
Second step, adjust pH
With the sodium hydroxide solution of weight percent concentration 4%, regulate said polynite slurry pH value to 9, obtain alkaline polynite slurry;
In the 3rd step, add octadecyl trimethyl ammonium chloride
Is that 55:1 mix with octadecyl trimethyl ammonium chloride according to weight part ratio with said alkaline polynite slurry, stirs, and obtains imvite modified mixture;
The 4th step, ball milling
Said imvite modified mixture is put into ball mill, and ball milling 8 hours obtains organic modification montmonrillonite;
The 5th step, oven dry
Said organic modification montmonrillonite is put into oven for drying, and 80 ℃ of temperature, obtain the exsiccant organic modification montmonrillonite at 18 hours time;
The 6th step, ball milling again
With said exsiccant organic modification montmonrillonite ball milling 0.5 hour once more in ball mill, sieve then, sieve aperture is 400 orders, obtains the finished product organic modification montmonrillonite.
Embodiment 6, and the organically-modified method of montmorillonite flame-retardant agent is carried out according to following steps:
The first step, slurrying
The deionized water of polynite with 70 ℃ mixed, stir, obtain the polynite slurry, the weight part ratio of said polynite and deionized water is 1:1.7;
Second step, adjust pH
With the sodium hydroxide solution of weight percent concentration 7%, regulate said polynite slurry pH value to 8, obtain alkaline polynite slurry;
In the 3rd step, add octadecyl trimethyl ammonium chloride
Is that 50:1 mix with octadecyl trimethyl ammonium chloride according to weight part ratio with said alkaline polynite slurry, stirs, and obtains imvite modified mixture;
The 4th step, ball milling
Said imvite modified mixture is put into ball mill, and ball milling 7 hours obtains organic modification montmonrillonite;
The 5th step, oven dry
Said organic modification montmonrillonite is put into oven for drying, and 72 ℃ of temperature, obtain the exsiccant organic modification montmonrillonite at 22 hours time;
The 6th step, ball milling again
With said exsiccant organic modification montmonrillonite ball milling 1 hour once more in ball mill, sieve then, sieve aperture is 270 orders, obtains the finished product organic modification montmonrillonite.
Embodiment 7, and the organically-modified method of montmorillonite flame-retardant agent is carried out according to following steps:
The first step, slurrying
The deionized water of polynite with 68 ℃ mixed, stir, obtain the polynite slurry, the weight part ratio of said polynite and deionized water is 1:1.2;
Second step, adjust pH
With the sodium hydroxide solution of weight percent concentration 5%, regulate said polynite slurry pH value to 9, obtain alkaline polynite slurry;
In the 3rd step, add octadecyl trimethyl ammonium chloride
Is that 40:1 mix with octadecyl trimethyl ammonium chloride according to weight part ratio with said alkaline polynite slurry, stirs, and obtains imvite modified mixture;
The 4th step, ball milling
Said imvite modified mixture is put into ball mill, and ball milling 6 hours obtains organic modification montmonrillonite;
The 5th step, oven dry
Said organic modification montmonrillonite is put into oven for drying, and 73 ℃ of temperature, obtain the exsiccant organic modification montmonrillonite at 20 hours time;
The 6th step, ball milling again
With said exsiccant organic modification montmonrillonite ball milling 1.5 hours once more in ball mill, sieve then, sieve aperture is 325 orders, obtains the finished product organic modification montmonrillonite.
Embodiment 8, and the organically-modified method of montmorillonite flame-retardant agent is carried out according to following steps:
The first step, slurrying
The deionized water of polynite with 67 ℃ mixed, stir, obtain the polynite slurry, the weight part ratio of said polynite and deionized water is 1:1.1;
Second step, adjust pH
With the sodium hydroxide solution of weight percent concentration 4%, regulate said polynite slurry pH value to 9, obtain alkaline polynite slurry;
In the 3rd step, add octadecyl trimethyl ammonium chloride
Is that 45:1 mix with octadecyl trimethyl ammonium chloride according to weight part ratio with said alkaline polynite slurry, stirs, and obtains imvite modified mixture;
The 4th step, ball milling
Said imvite modified mixture is put into ball mill, and ball milling 5 hours obtains organic modification montmonrillonite;
The 5th step, oven dry
Said organic modification montmonrillonite is put into oven for drying, and 75 ℃ of temperature, obtain the exsiccant organic modification montmonrillonite at 16 hours time;
The 6th step, ball milling again
With said exsiccant organic modification montmonrillonite ball milling 1.8 hours once more in ball mill, sieve then, sieve aperture is 400 orders, obtains the finished product organic modification montmonrillonite.
Embodiment 9, and the organically-modified method of montmorillonite flame-retardant agent is carried out according to following steps:
The first step, slurrying
The deionized water of polynite with 68 ℃ mixed, stir, obtain the polynite slurry, the weight part ratio of said polynite and deionized water is 1:1.8;
Second step, adjust pH
With the sodium hydroxide solution of weight percent concentration 7%, regulate said polynite slurry pH value to 9, obtain alkaline polynite slurry;
In the 3rd step, add octadecyl trimethyl ammonium chloride
Is that 38:1 mix with octadecyl trimethyl ammonium chloride according to weight part ratio with said alkaline polynite slurry, stirs, and obtains imvite modified mixture;
The 4th step, ball milling
Said imvite modified mixture is put into ball mill, and ball milling 7 hours obtains organic modification montmonrillonite;
The 5th step, oven dry
Said organic modification montmonrillonite is put into oven for drying, and 74 ℃ of temperature, obtain the exsiccant organic modification montmonrillonite at 21 hours time;
The 6th step, ball milling again
With said exsiccant organic modification montmonrillonite ball milling 0.8 hour once more in ball mill, sieve then, sieve aperture is 230 orders, obtains the finished product organic modification montmonrillonite.
Embodiment 10, and the organically-modified method of montmorillonite flame-retardant agent is carried out according to following steps:
The first step, slurrying
The deionized water of polynite with 80 ℃ mixed, stir, obtain the polynite slurry, the weight part ratio of said polynite and deionized water is 1:1.5;
Second step, adjust pH
With the sodium hydroxide solution of weight percent concentration 4%, regulate said polynite slurry pH value to 8, obtain alkaline polynite slurry;
In the 3rd step, add octadecyl trimethyl ammonium chloride
Is that 48:1 mix with octadecyl trimethyl ammonium chloride according to weight part ratio with said alkaline polynite slurry, stirs, and obtains imvite modified mixture;
The 4th step, ball milling
Said imvite modified mixture is put into ball mill, and ball milling 8 hours obtains organic modification montmonrillonite;
The 5th step, oven dry
Said organic modification montmonrillonite is put into oven for drying, and 79 ℃ of temperature, obtain the exsiccant organic modification montmonrillonite at 22 hours time;
The 6th step, ball milling again
With said exsiccant organic modification montmonrillonite ball milling 2 hours once more in ball mill, sieve then, sieve aperture is 400 orders, obtains the finished product organic modification montmonrillonite.
Claims (2)
1. the organically-modified method of montmorillonite flame-retardant agent is characterized in that carrying out according to following steps:
The first step, slurrying
The deionized water of polynite with 60 ℃-85 ℃ mixed, stir, obtain the polynite slurry, the weight part ratio of said polynite and deionized water is 1:0.5-2;
Second step, adjust pH
With the sodium hydroxide solution of weight percent concentration 3%-8%, regulate said polynite slurry pH value to 8-9, obtain alkaline polynite slurry;
In the 3rd step, add cation modifier
Is that 30-60:1 mix with cation modifier according to weight part ratio with said alkaline polynite slurry, stirs, and obtains imvite modified mixture;
The 4th step, ball milling
Said imvite modified mixture is put into ball mill, ball milling 4-8 hour, obtain organic modification montmonrillonite;
The 5th step, oven dry
Said organic modification montmonrillonite is put into oven for drying, and 70 ℃-80 ℃ of temperature time 15-25 hour, obtain the exsiccant organic modification montmonrillonite;
The 6th step, ball milling again
With said exsiccant organic modification montmonrillonite in ball mill ball milling 0.5-2 hour once more, sieve then, sieve aperture is the 200-400 order, obtains the finished product organic modification montmonrillonite.
2. the organically-modified method of montmorillonite flame-retardant agent according to claim 1 is characterized in that described cation modifier is an octadecyl trimethyl ammonium chloride.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104211076A (en) * | 2013-06-04 | 2014-12-17 | 中国地质大学（北京） | Semidry method for preparation of organic intercalated type montmorillonite |
| CN104211076B (en) * | 2013-06-04 | 2016-05-11 | 中国地质大学（北京） | Be prepared with the semidry method of machine transplanting of rice stratotype montmorillonite |
| CN111793459A (en) * | 2020-06-22 | 2020-10-20 | 安徽南大星新材料科技有限公司 | Novel flame-retardant low-shrinkage polyurethane foam joint mixture |
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Application publication date: 20120215 |