CN1253164A - Process for preparing polycondensation-type flame-retarding high-molecular/nm-class SiO2 compound material - Google Patents
Process for preparing polycondensation-type flame-retarding high-molecular/nm-class SiO2 compound material Download PDFInfo
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- CN1253164A CN1253164A CN 98114449 CN98114449A CN1253164A CN 1253164 A CN1253164 A CN 1253164A CN 98114449 CN98114449 CN 98114449 CN 98114449 A CN98114449 A CN 98114449A CN 1253164 A CN1253164 A CN 1253164A
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Abstract
A polycondensation-type flame-retarding high-molecular/nm-class SiO2 compound material is prepared through sol-gel reaction, where ethyl n-silicate is hydrolyzed by water generated by polycondensation-type high-molecular synthesis reaction. The size of SiO2 particle can be controlled in tens of nm with uniform granularities. Its advantages are simple preparing process, and intensified flame-retarding and thermal properties. When it burns, no smoke and toxin are released.
Description
The present invention relates to the preparation method of flame-proof composite material.Specifically a kind of condensation polymer type macromolecule/nano SiO
2The preparation of flame-proof composite material, this matrix material can have the thermal characteristics of reinforced flame retardant under the situation that keeps mechanical property.
Macromolecular material is because light weight, specific tenacity are big, and especially some special material has high thermal resistance preferably, electrical insulating property and being widely used.But easily burning is the most outstanding shortcoming of macromolecular material, and therefore the fire-retardant fireproof that improves macromolecular material more and more higher today in fire-retardant requirement has become an important topic of macromolecular material research.Wherein inorganic materials being dispersed in and forming inorganic-polymer composite in the macromolecular material owing to smokelessly nontoxic when burning, be better than traditional Halogen flame retarded polymeric material, is the effective ways that improve flame retardant resistance.Reported in literature is inorganic-and the preparation method of polymer composite is a physical blending, the granular size of inorganic materials and size distribution have considerable influence to mechanical property, thermal characteristics and the flame retardant properties of material, therefore with inorganic materials super-strengthening, homogenizing in the polymer, improving its flame retardant resistance and thermal characteristics is that people very pay close attention to.
The purpose of this invention is to provide a kind of polymer composite with better fire-retardant fireproof performance, and provide its preparation method, this flame-proof composite material has the thermal characteristics of higher flame retardant resistance.
Preparation method provided by the invention is not inorganic materials and high molecular simple physical blend, and nanometer SiO
2Be by sol gel reaction, utilize the water hydrolysis tetraethoxy that generates in the condensation polymer type macromolecular synthetic reaction process to obtain, this method can make SiO
2The particle diameter uniform distribution, and be controlled at tens nanometers with interior (less than 100 nanometers).And, help the carrying out of polyreaction owing to utilized the water that generates in the polymerization process.
Condensation polymer type macromolecule/nano SiO provided by the invention
2Matrix material comprises condensation polymer type polymer and nanometer SiO
2The condensation polymer type polymer is polyester, polyimide, polysulfones, polymeric amide, polybenzimidazole pyrrolidone, polybenzothiozole and polybenzimidazole etc.; Nanometer SiO
2Weight percentage is 2～50% in matrix material, and optimum range is 3～20%.Condensation polymer type macromolecule/nano SiO provided by the invention
2Matrix material can have the thermal characteristics and the flame retardant properties of raising under the prerequisite that keeps mechanical property.
Condensation polymer type macromolecule/nano SiO provided by the invention
2The preparation method of matrix material can be according to the following steps:
1. synthetic macromolecule polycondensate
Polycondensation technology is routinely carried out.
2. condensation polymer type macromolecule/nano SiO
2The preparation of matrix material
Add a certain amount of (2～50%) tetraethoxy in polycondensation process, sol gel reaction and polycondensation are carried out simultaneously.
Below by embodiment to condensation polymer type macromolecule/nano SiO provided by the invention
2Matrix material is described further.
Embodiment
1. the condensation polymer type polyphosphazene polymer is imido synthetic
Diamines yl diphenyl ether 31.39g is dissolved in the 336g N,N-dimethylacetamide, add 3,3 in batches ', 4,4 '-benzophenone tetracarboxylic dianhydride 50g, stirred 6 hours under the room temperature, synthetic solid content is 20% polyamic acid solution.
2.SiO
2Content is polyimide/nanometer SiO of 3～19%
2The preparation of matrix material
Respectively embodiment 1～4 required tetraethoxy amount and the 12g polyamic acid solution that provides in the table 1 stirred 12 hours together.Then solution is filmed on sheet glass.Slowly be warmed up to 100 ℃, under 100 ℃, 200 ℃ and 300 ℃, respectively heated 1 hour then.Obtain SiO
2Content is polyimide/nanometer SiO of 0～19%
2Matrix material.
3. polyimide/nanometer SiO
2The physicals of matrix material
Table 1 polyimide/nanometer SiO
2The physicals of matrix material
Example 1 example 2 examples 3 example 4SiO
2Wt% 3 10 15 19 second-order transition temperatures ℃ 280 279 285 2855% thermal weight loss temperature ℃ 520 515 520 518 oxygen indexs, 30 32 37 37 tensile strength MPa 110 112 106 119
By the foregoing description, condensation polymer type macromolecule/nano SiO provided by the invention
2The preparation method of matrix material can make SiO
2Grain diameter is tens nanometers, and size distribution is even.This material has reinforced flame retardant and thermal characteristics under the prerequisite that keeps mechanical property, smokelessly nontoxic during fuel.This preparation method's technology is simple, is suitable for using.
Claims (3)
1. condensation polymer type macromolecule/nano SiO
2The preparation method of flame-proof composite material is characterized in that nanometer SiO
2Be by sol gel reaction, utilize the water hydrolysis tetraethoxy that generates in the condensation polymer type macromolecular synthetic reaction process to obtain.
2. by the described condensation polymer type macromolecule/nano of claim 1 SiO
2The preparation method of flame-proof composite material is characterized in that condensation polymer type polymer wherein is polyester, polyimide, polysulfones, polymeric amide, polybenzimidazole pyrrolidone, polybenzothiozole and polybenzimidazole etc.
3. by the described condensation polymer type macromolecule/nano of claim 1 SiO
2The preparation method of flame-proof composite material is characterized in that nanometer SiO wherein
2Weight percentage is 3～20%, SiO
2Particle diameter can be controlled in tens nanometers.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98114449 CN1129661C (en) | 1998-11-11 | 1998-11-11 | Process for preparing polycondensation-type flame-retarding high-molecular/nm-class SiO2 compound material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98114449 CN1129661C (en) | 1998-11-11 | 1998-11-11 | Process for preparing polycondensation-type flame-retarding high-molecular/nm-class SiO2 compound material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1253164A true CN1253164A (en) | 2000-05-17 |
| CN1129661C CN1129661C (en) | 2003-12-03 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 98114449 Expired - Fee Related CN1129661C (en) | 1998-11-11 | 1998-11-11 | Process for preparing polycondensation-type flame-retarding high-molecular/nm-class SiO2 compound material |
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| CN (1) | CN1129661C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103013120A (en) * | 2011-09-28 | 2013-04-03 | 深圳光启高等理工研究院 | Nano-composite flame retardant material and preparation method thereof |
-
1998
- 1998-11-11 CN CN 98114449 patent/CN1129661C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103013120A (en) * | 2011-09-28 | 2013-04-03 | 深圳光启高等理工研究院 | Nano-composite flame retardant material and preparation method thereof |
| CN103013120B (en) * | 2011-09-28 | 2015-02-04 | 深圳光启高等理工研究院 | Nano-composite flame retardant material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1129661C (en) | 2003-12-03 |
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