CN101307182A - Method for preparing meso-scale flaky vermiculite and heat-resistant polymer heat insulation composite membrane - Google Patents
Method for preparing meso-scale flaky vermiculite and heat-resistant polymer heat insulation composite membrane Download PDFInfo
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- CN101307182A CN101307182A CNA2008100396554A CN200810039655A CN101307182A CN 101307182 A CN101307182 A CN 101307182A CN A2008100396554 A CNA2008100396554 A CN A2008100396554A CN 200810039655 A CN200810039655 A CN 200810039655A CN 101307182 A CN101307182 A CN 101307182A
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Abstract
The invention provides a method for preparing mesoscale flaky vermiculite and high temperature polymer thermal insulation composite membrane. The invention adopts a technical proposal that primary mineral of vermiculite are ground to choose the part of vermiculite with a grain diameter less than 10 mu m; quaternary alkylammonium salt compound with a carbon chain of between 12 and 36 is used to modify the chosen vermiculite by organic expansion; a dispersing agent, grinding and a high-pressure homogenizer are adopted to treat the mesoscale flaky vermiculite; inorganic flaky vermiculite microcrystals are dispersed in organic high molecular polymer materials by using high temperature resistance polymer materials of poly(aryl ether sulfone) and poly(phthalazinone ether sulfone ketone) as continuous phrases and by methods of ultrasonic cell disruption, etc., and are formed into membranes by dry and wet methods. The products made by the method have extremely low heat conductivity, and excellent thermal insulation performance. Meanwhile, the composite membrane can be tightly covered on the surfaces of polysulfonamide and other fiber fabrics to improve the fireproof and thermal insulation properties, particularly the thermal insulation property of the fiber fabrics, can be used to make fire-protection clothing for safe access to fire ground or used as surface material for combat uniform.
Description
Technical field
The present invention relates to the preparation method of a kind of meso-scale flaky vermiculite and heat-resistant polymer heat insulation composite membrane.
Background technology
The method that fabric fire-proof and thermal-insulation ideal method is to use coating forms a thermofin at fabric with extraneous, the effect of thermofin be prevent heat import into by except the space, its main characteristic that should have is: thermal conductivity is little, capacity is little, high thermal resistance is good.
Thermal conductivity k is one of physical properties of material.The power of the size reflection material capacity of heat transmission of its value, its value is big more, and the capacity of heat transmission is strong more.Usually select suitable thermally conductive material according to the numerical value of thermal conductivity, the occasion that need reduce heat conduction speed is selected the little material of thermal conductivity for use.
And original high-temperature polymer material is polyether sulphone (being designated hereinafter simply as PES), its thermal conductivity is 0.086/mk or assorted naphthalene biphenyl polyether sulfone ketone (being designated hereinafter simply as PPESK), its thermal conductivity is 0.076/mk, their heat-proof quality is all bad, has limited their application on lagging material.
Hydrous micas ore deposit---vermiculite can satisfy above-mentioned most requirement, possess little, the heat insulation good characteristics of thermal conductivity, and at decomposition, dehydration, the generation rare gas element of chemical substance the minimizing of material surface oxygen level, distillation and the width of cloth are penetrated etc. under the situation still to demonstrate its protective characteristic.It can not increase weight to structure, can guarantee that again the material that mechanize is produced has resistivity against fire efficiently simultaneously.
Summary of the invention
The preparation method who the purpose of this invention is to provide the lower lagging material of a kind of thermal conductivity.In order to achieve the above object, the invention provides the preparation method of a kind of meso-scale flaky vermiculite and heat-resistant polymer heat insulation composite membrane.
Know-why of the present invention is: by inorganic cation between vermiculite layers and-ium compound ion exchange effect, increase the vermiculite layers spacing, prepare the flaky vermiculite of meso-scale again in conjunction with means such as physical grinding and high pressure microjet homogeneous.Use dry method and wet method with inorganic meso-scale flaky vermiculite and high-temperature polymer composite membrane-forming again, utilize the resistance to elevated temperatures of inorganic vermiculite,, improve the anti-naked light and the heat-proof quality of high-temperature polymer material membrane thermal-radiating reflection/sorption.
Concrete steps of the present invention are:
Step 1, primary mineral of vermiculite grind 2h～100h, filter out the vermiculite of particle diameter less than 10um, seasoning;
Step 2, the vermiculite that step 1 is prepared soak the pool in redistilled water, the quaternary ammonium alkyl salt compound that adds the consumption of 1～8 times of cationic exchange, under 50 ℃～80 ℃ temperature condition, stirring reaction 6h～100h carries out the organic expander modification to the vermiculite that screens;
Step 3, the vermiculite for preparing with deionized water repetitive scrubbing step 2 are up to no Br
-, Cl
-There is seasoning subsequently;
Step 4, be 100%, soak the pool in 10～50 times redistilled water, add dispersion agent 20%～100% again in the vermiculite weight that obtains by step 3; Described dispersion agent is sodium lauryl sulphate or dispersion agent FZ or Sodium hexametaphosphate 99 etc.;
Step 5, the vermiculite aqueous dispersion that step 4 is prepared grind 2h～100h, handle 1 time～50 times with high pressure microjet homogenizer subsequently, and centrifugal, vacuum-drying 24h～168h makes meso-scale flaky vermiculite;
Step 6, with N-Methyl pyrrolidone, N, a kind of and butyl glycol ether and butanone in dinethylformamide or the N,N-dimethylacetamide stir at normal temperatures and pressures, obtain mixed solvent;
The weight of step 7, the mixed solvent for preparing in step 6 is 100%, at normal temperatures and pressures, adds high-temperature polymer polyether sulphone or assorted naphthalene biphenyl polyether sulfone ketone 10%～30% in described mixing solutions, soaks damp 1h～24h, and it is fully dissolved;
Step 8, be 100% in the high-temperature polymer polyether sulphone that adds in the step 7 or the weight of assorted naphthalene biphenyl polyether sulfone ketone, in polyether sulphone that step 7 prepares or assorted naphthalene biphenyl polyether sulfone ketoboidies system, add the meso-scale flaky vermiculite that 15%～25% step 5 prepares, utilize ultrasonic cell disruptor subsequently, under 450w～550w power condition, supersound process 5 times～20 times, time 50s～200s makes it uniform mixing altogether, makes film-casting liquid;
Step 9, will spread upon by the film-casting liquid that step 8 obtains on the sheet glass, and use conventional dry method or wet method to prepare meso-scale flaky vermiculite and heat-resistant polymer heat insulation composite membrane.
Further, the disintegrating apparatus described in step 1 and the step 5 is sand mill or basket shredder or pulverizing mill or ball mill etc.
Quaternary ammonium alkyl salt compound described in the step 2 is Dodecyl trimethyl ammonium chloride or cetyl trimethylammonium bromide or INCROQUAT TMC-80 or two octadecyl trimethyl ammonium chloride etc.
The proportioning of the mixed solvent described in the step 6 is, weight with mixed solvent is 100% note, N-Methyl pyrrolidone or N, dinethylformamide or N, the N-N,N-DIMETHYLACETAMIDE is 50%～90%, butyl glycol ether be 5%～20% and butanone be 5%～30%.
The invention has the beneficial effects as follows: meso-scale flaky vermiculite and its thermal conductivity of high-temperature polymer composite membrane of making by the present invention are extremely low, have good heat-proof quality.Composite membrane can closely be coated on fabric surface such as fragrant sulfone synthetic fibre simultaneously, improves its anti-naked light, thermal isolation performance, and particularly the thermal isolation performance can be used for can come in and go out the safely bunker clothing in the scene of a fire or the cladding material of fighting uniform.Achievement in research of the present invention can also be used to improve the resistance toheat of common organic fibrous materials such as polycaprolactam 6, improves the maximum operation (service) temperature of such material, realizes the high performance of common high molecular materials.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, claims institute restricted portion that falls within the application is equally changed or revised to the equivalent form of value.
Embodiment 1
Can be divided into following steps referring to Fig. 1 the present invention:
Step 1, be that the zirconia ball of 2～3mm carries out sand milling 8h to primary mineral of vermiculite in sand mill, filter out the vermiculite of particle diameter subsequently, seasoning again less than 10um with diameter;
Step 2, will soak the pool by the vermiculite that step 1 obtains in redistilled water, and add the Dodecyl trimethyl ammonium chloride of the consumption of 4 times of cationic exchange, under 80 ℃ temperature condition, stirring reaction 6h carries out the organic expander modification to the vermiculite of screening;
Step 3, the vermiculite that obtains by step 2 with the deionized water repetitive scrubbing are up to no Br
-, Cl
-There is seasoning subsequently;
Step 4, be 100%, soak the pool in 20 times redistilled water, add sodium lauryl sulphate 20% again in the vermiculite weight that obtains by step 3;
Step 5, be that the zirconia ball of 1mm grinds 8h to the vermiculite aqueous dispersion that obtains by step 4 in sand mill, handle 10 times with high pressure microjet homogenizer subsequently that centrifugal, vacuum-drying 24h makes meso-scale flaky vermiculite with diameter;
Step 6, N-Methyl pyrrolidone and butyl glycol ether and butanone are stirred at normal temperatures and pressures, obtain mixed solvent; The proportioning of described mixed solvent is, is 100% note with the weight of mixed solvent, and N-Methyl pyrrolidone is 78%, butyl glycol ether be 5% and butanone be 17%;
Step 7, be 100%, at normal temperatures and pressures, high-temperature polymer PES10% soaked the pool in the mixed solvent that obtains by step 6, soak damp 12h, it fully is dissolved in the described mixed solvent in the weight of the mixed solvent for preparing by step 6;
Step 8, be 100% in the weight of the high-temperature polymer PES that adds in the step 7, the meso-scale flaky vermiculite 20% that adding prepares by step 5 is in the PES system, utilize ultrasonic cell disruptor subsequently, under the 500w power condition, supersound process 10 times, time 100s makes it uniform mixing altogether, makes film-casting liquid;
Step 9, will spread upon by the film-casting liquid that step 8 obtains on the sheet glass, and use conventional dried preparation to obtain meso-scale flaky vermiculite and heat-resistant polymer heat insulation composite membrane.Recording its thermal conductivity is 0.038W/mk.
Embodiment 2
Step 1, primary mineral of vermiculite is ground 100h, filter out the vermiculite of particle diameter subsequently, seasoning again less than 10um with basket shredder;
Step 2, will soak the pool by the vermiculite that step 1 obtains in redistilled water, and add the cetyl trimethylammonium bromide of the consumption of 8 times of cationic exchange, under 50 ℃ temperature condition, stirring reaction 100h carries out the organic expander modification to the vermiculite of screening;
Step 3, the vermiculite that obtains by step 2 with the deionized water repetitive scrubbing are up to no Br
-, Cl
-There is seasoning subsequently;
Step 4, be 100%, soak the pool in 10 times redistilled water, add dispersion agent FZ100% again in the vermiculite weight that obtains by step 3;
Step 5, with basket shredder the vermiculite aqueous dispersion that obtains by step 4 is ground 2h, handle 50 times with high pressure microjet homogenizer subsequently, centrifugal, vacuum-drying 96h makes meso-scale flaky vermiculite;
Step 6, with N, dinethylformamide and butyl glycol ether and butanone stir at normal temperatures and pressures, obtain mixed solvent; The proportioning of described mixed solvent is, is 100% note with the weight of mixed solvent, and N, dinethylformamide are 90%, butyl glycol ether be 5% and butanone be 5%;
Step 7, be 100%, at normal temperatures and pressures, high-temperature polymer PES20% soaked the pool in the mixed solvent that obtains by step 6, soak damp 1h, it fully is dissolved in the described mixed solvent in the weight of the mixed solvent for preparing by step 6;
Step 8, be 100% in the weight of the high-temperature polymer PES that adds in the step 7, the meso-scale flaky vermiculite 15% that adding prepares by step 5 is in the PES system, utilize ultrasonic cell disruptor subsequently, under the 450w power condition, supersound process 20 times, time 200s makes it uniform mixing altogether, makes film-casting liquid;
Step 9, will spread upon by the film-casting liquid that step 8 obtains on the sheet glass, and use conventional wet method to prepare meso-scale flaky vermiculite and heat-resistant polymer heat insulation composite membrane.Recording its thermal conductivity is 0.045W/mk.
Embodiment 3
Step 1, primary mineral of vermiculite is ground 2h, filter out the vermiculite of particle diameter subsequently, seasoning again less than 10um with pulverizing mill;
Step 2, will soak the pool by the vermiculite that step 1 obtains in redistilled water, and add the INCROQUAT TMC-80 of the consumption of 1 times of cationic exchange, under 80 ℃ temperature condition, stirring reaction 12h carries out the organic expander modification to the vermiculite of screening;
Step 3, the vermiculite that obtains by step 2 with the deionized water repetitive scrubbing are up to no Br
-, Cl
-There is seasoning subsequently;
Step 4, be 100%, soak the pool in 30 times redistilled water, add Sodium hexametaphosphate 99 30% again in the vermiculite weight that obtains by step 3;
Step 5, with pulverizing mill the vermiculite that obtains by step 4 is ground 100h, handle 1 time with high pressure microjet homogenizer subsequently, centrifugal, vacuum-drying 48h makes meso-scale flaky vermiculite;
Step 6, N,N-dimethylacetamide and butyl glycol ether and butanone are stirred at normal temperatures and pressures, obtain mixed solvent; The proportioning of described mixed solvent is, is 100% in the weight of mixed solvent, and N,N-dimethylacetamide is 50%, butyl glycol ether be 20% and butanone be 30%;
Step 7, be 100%, at normal temperatures and pressures, high-temperature polymer PPESK10% soaked the pool in the mixed solvent that obtains by step 6, soak damp 12h, it fully is dissolved in the described mixed solvent in the weight of the mixed solvent for preparing by step 6;
Step 8, be 100% in the weight of the high-temperature polymer PPESK that adds in the step 7, the meso-scale flaky vermiculite 25% that adding prepares by step 5 is in the PPESK system, utilize ultrasonic cell disruptor subsequently, under the 550w power condition, supersound process 5 times, time 50s makes it uniform mixing altogether, makes film-casting liquid;
Step 9, will spread upon by the film-casting liquid that step 8 obtains on the sheet glass, and use conventional dried preparation to obtain meso-scale flaky vermiculite and heat-resistant polymer heat insulation composite membrane.Recording its thermal conductivity is 0.041W/mk.
Embodiment 4
Step 1, primary mineral of vermiculite is carried out sand milling 50h, filter out the vermiculite of particle diameter subsequently, seasoning again less than 10um with ball mill;
Step 2, will soak the pool by the vermiculite that step 1 obtains in redistilled water, and add two octadecyl trimethyl ammonium chloride of the consumption of 4 times of cationic exchange, under 80 ℃ temperature condition, stirring reaction 8h carries out the organic expander modification to the vermiculite that screens;
Step 3, the vermiculite that obtains by step 2 with the deionized water repetitive scrubbing are up to no Br
-, Cl
-There is seasoning subsequently;
Step 4, be 100%, soak the pool in 20 times redistilled water, add sodium lauryl sulphate 20% again in the vermiculite weight that obtains by step 3;
Step 5, with ball mill the vermiculite that obtains by step 4 is ground 50h, handle 20 times with high pressure microjet homogenizer subsequently, centrifugal, vacuum-drying 168h makes meso-scale flaky vermiculite;
Step 6, N-Methyl pyrrolidone and butyl glycol ether and butanone are stirred at normal temperatures and pressures, obtain mixed solvent; The proportioning of described mixed solvent is, is 100% note with the weight of mixed solvent, and N-Methyl pyrrolidone is 78%, butyl glycol ether be 5% and butanone be 17%;
Step 7, be 100%, at normal temperatures and pressures, high-temperature polymer PPESK30% soaked the pool in the mixed solvent that obtains by step 6, soak damp 24h, it fully is dissolved in the described mixed solvent in the weight of the mixed solvent for preparing by step 6;
Step 8, be 100% in the weight of the high-temperature polymer PPESK that adds in the step 7, the meso-scale flaky vermiculite 15% that adding prepares by step 5 is in the PPESK system, utilize ultrasonic cell disruptor subsequently, under the 500w power condition, supersound process 10 times, time 100s makes it uniform mixing altogether, makes film-casting liquid;
Step 9, will spread upon by the film-casting liquid that step 8 obtains on the sheet glass, and use conventional dried preparation to obtain meso-scale flaky vermiculite and heat-resistant polymer heat insulation composite membrane.Recording its thermal conductivity is 0.047W/mk.
By the heat flow method of routine, can record the data in the following table
The performance synopsis
| Thermal conductivity (W/mk) | Thermal conductivity (W/mk) | ||
| Do not implement present method PES | 0.086 | Do not implement present method PPESK | 0.076 |
| Embodiment 1 | 0.038 | Embodiment 3 | 0.041 |
| Embodiment 2 | 0.045 | Embodiment 4 | 0.047 |
Claims (4)
1. the preparation method of meso-scale flaky vermiculite and heat-resistant polymer heat insulation composite membrane is characterized in that, comprises the following steps:
Step 1, primary mineral of vermiculite grind 2h～100h, filter out the vermiculite of particle diameter less than 10 μ m, seasoning;
Step 2, the vermiculite that step 1 is prepared soak the pool in redistilled water, the quaternary ammonium alkyl salt compound that adds 1～8 times of cationic exchange consumption, under 50 ℃～80 ℃ temperature condition, more than the stirring reaction 6h, the vermiculite that screens is carried out the organic expander modification;
Step 3, the vermiculite for preparing with deionized water repetitive scrubbing step 2 are up to no Br
-, Cl
-There is seasoning subsequently;
Step 4, the vermiculite weight for preparing in step 3 are 100%, soak the pool in 10～50 times redistilled water, add dispersion agent 20%～100% again;
Step 5, the vermiculite aqueous dispersion that step 4 is prepared grind 2h～100h, handle 1 time～50 times with high pressure microjet homogenizer subsequently, and centrifugal, vacuum-drying 24h～168h makes meso-scale flaky vermiculite;
Step 6, with N-Methyl pyrrolidone, N, a kind of and butyl glycol ether and butanone in dinethylformamide or the N,N-dimethylacetamide stir at normal temperatures and pressures, obtain mixed solvent;
The weight of step 7, the mixed solvent for preparing in step 6 is 100%, at normal temperatures and pressures, adds high-temperature polymer polyether sulphone or assorted naphthalene biphenyl polyether sulfone ketone 10%～30% in described mixing solutions, soaks damp 1h～24h, and it is fully dissolved;
Step 8, be 100% in the high-temperature polymer polyether sulphone that adds in the step 7 or the weight of assorted naphthalene biphenyl polyether sulfone ketone, in polyether sulphone that step 7 prepares or assorted naphthalene biphenyl polyether sulfone ketoboidies system, add the meso-scale flaky vermiculite that 15%～25% step 5 prepares, utilize ultrasonic cell disruptor subsequently, under 450w～550w power condition, supersound process 5 times～20 times, time 50s～200s makes it uniform mixing altogether, makes film-casting liquid;
Step 9, the film-casting liquid that step 8 is prepared spread upon on the sheet glass, use conventional dry method or wet method to prepare meso-scale flaky vermiculite and heat-resistant polymer heat insulation composite membrane.
2. the preparation method of meso-scale flaky vermiculite as claimed in claim 1 and heat-resistant polymer heat insulation composite membrane, it is characterized in that the quaternary ammonium alkyl salt compound described in the step 2 is a kind of in Dodecyl trimethyl ammonium chloride or cetyl trimethylammonium bromide or INCROQUAT TMC-80 or the two octadecyl trimethyl ammonium chloride.
3. the preparation method of meso-scale flaky vermiculite as claimed in claim 1 and heat-resistant polymer heat insulation composite membrane is characterized in that, the dispersion agent described in the step 4 is sodium lauryl sulphate or dispersion agent FZ or Sodium hexametaphosphate 99.
4. the preparation method of meso-scale flaky vermiculite as claimed in claim 1 and heat-resistant polymer heat insulation composite membrane, it is characterized in that, the weight proportion of the mixed solvent described in the step 6 is, N-Methyl pyrrolidone or N, dinethylformamide or N, the N-N,N-DIMETHYLACETAMIDE is 50%～90%, butyl glycol ether be 5%～20% and butanone be 5%～30%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070154A (en) * | 2010-12-07 | 2011-05-25 | 东华大学 | Preparation method of inorganic vermiculite film |
| CN102503482A (en) * | 2011-11-03 | 2012-06-20 | 武汉科技大学 | Low-thermal conductivity modified vermiculite composite thermal insulation material and preparation method thereof |
| CN102992651A (en) * | 2012-11-13 | 2013-03-27 | 西安友基复合材料有限公司 | Method for coating emulsion for fireproof insulation fiberglass |
| CN103114433A (en) * | 2013-03-05 | 2013-05-22 | 南通大学 | Preparation method of open-fire resistance thermal insulation textile |
| CN105694110A (en) * | 2016-01-26 | 2016-06-22 | 中南林业科技大学 | Aperture-adjustable cellulose and montmorillonite nano-composite carrier material and preparation method thereof |
| CN116063866A (en) * | 2023-01-10 | 2023-05-05 | 东莞希乐斯科技有限公司 | Vermiculite-based composite flame retardant and preparation method thereof |
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2008
- 2008-06-26 CN CN2008100396554A patent/CN101307182B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070154A (en) * | 2010-12-07 | 2011-05-25 | 东华大学 | Preparation method of inorganic vermiculite film |
| CN102070154B (en) * | 2010-12-07 | 2013-01-02 | 东华大学 | Preparation method of inorganic vermiculite film |
| CN102503482A (en) * | 2011-11-03 | 2012-06-20 | 武汉科技大学 | Low-thermal conductivity modified vermiculite composite thermal insulation material and preparation method thereof |
| CN102503482B (en) * | 2011-11-03 | 2013-07-10 | 武汉科技大学 | Low-thermal conductivity modified vermiculite composite thermal insulation material and preparation method thereof |
| CN102992651A (en) * | 2012-11-13 | 2013-03-27 | 西安友基复合材料有限公司 | Method for coating emulsion for fireproof insulation fiberglass |
| CN103114433A (en) * | 2013-03-05 | 2013-05-22 | 南通大学 | Preparation method of open-fire resistance thermal insulation textile |
| CN105694110A (en) * | 2016-01-26 | 2016-06-22 | 中南林业科技大学 | Aperture-adjustable cellulose and montmorillonite nano-composite carrier material and preparation method thereof |
| CN105694110B (en) * | 2016-01-26 | 2018-08-14 | 中南林业科技大学 | A kind of adjustable cellulose in aperture and montmorillonite-based nano composite carrier and preparation method thereof |
| CN116063866A (en) * | 2023-01-10 | 2023-05-05 | 东莞希乐斯科技有限公司 | Vermiculite-based composite flame retardant and preparation method thereof |
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