CN101291878A - Thermally stable aluminum hydroxide particles and their use as fillers in epoxy laminate resins - Google Patents

Thermally stable aluminum hydroxide particles and their use as fillers in epoxy laminate resins Download PDF

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CN101291878A
CN101291878A CNA2006800386477A CN200680038647A CN101291878A CN 101291878 A CN101291878 A CN 101291878A CN A2006800386477 A CNA2006800386477 A CN A2006800386477A CN 200680038647 A CN200680038647 A CN 200680038647A CN 101291878 A CN101291878 A CN 101291878A
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ath
scope
tga
flame
retardant resin
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勒内·赫尔比特
因戈·海姆
诺贝特·W.·皮茨
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Albemarle Corp
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract

Aluminum hydroxide particles having improved thermal stability and their use as a flame retardant in resins suitable for use in epoxy laminates, and laminates containing the same.

Description

Thermally stable aluminum hydroxide particles and they in epoxy laminate resins as the purposes of filler
The cross reference of related application
The application requires the U.S. Provisional Application 60/816,455 of submission early and 60/728,199 right, and they are attached to herein as a reference in full.
Invention field
The present invention relates to the purposes of granular aluminium hydroxide.More specifically, the present invention relates to the purposes of the aluminum hydroxide particles of thermostability raising as fire retardant.
Background of invention
Aluminium hydroxide has many selectable titles, the for example hydrate of aluminium (aluminum hydrate), aluminum trihydrate (aluminum trihydrate), three aluminium hydroxides (aluminum trihydroxide) etc., but be commonly referred to ATH, thereby this paper adopts ATH.The ATH particle is used as filler in many materials such as paper, resin, rubber, plastics etc.These products are used for different commercial applications, for example cable and wire sheath, travelling belt, thermoplastic mould, tackiness agent etc.The ATH particle typically is used to improve the flame retardant resistance of these materials, also serves as smoke suppressant.
Because adopting in the application of ATH usually, the final user monitors the thermostability of ATH closely.For example, in printed circuit board applications, the thermostability that is used to constitute the laminating material of plate must be enough high, with the permission pb-free solder.Therefore, this area need have the ATH of the thermostability of improvement.
The accompanying drawing summary
Fig. 1 is that comparison is according to the figure of aluminium hydroxide of the present invention with the thermostability of the existing aluminium hydroxide that can buy.
Fig. 2 describes to contain with good grounds ATH of the present invention, Martinal
Figure A20068003864700071
OL-104/WE and Martinal OL-104/LE reaches the figure of stratified mean time as the preparation of epoxy resin laminates of filler.
Summary of the invention
The inventor finds unexpectedly that in this thermostability of ATH is relevant with the soda of ATH (soda) content.Although it is relevant with total sodiun carbomate inventory of ATH that experimental evidence shows thermostability, do not wish to be bound by theory, the inventor thinks that in this thermostability of ATH raising of the present invention is relevant with the content of soluble soda, based on total soda, the content of this soluble soda typically is about 70 of total sodiun carbomate inventory and arrives in the scope of about 99wt%, and surplus is solvable soda.Therefore, the present invention relates to flame-retardant resin formulation, it comprise have one or more, the preferred two or more and more preferably ATH:d of three kinds or how following feature 10From about 0.5 in the scope of about 1.4 μ m; d 50From about 1.2 in the scope of about 3.0 μ m; d 90From about 2.2 in the scope of about 6.0 μ m; Based on ATH, less than total sodiun carbomate inventory of about 0.2wt%, the Toenol 1140 oil number of measuring according to ISO787-5:1980 is in about scope of 15 to about 40ml/100g; And the specific surface area of measuring according to DIN-66132 (BET) from about 2.0 to about 8m 2In/g the scope, wherein the electric conductivity of ATH is less than about 200 μ S/cm, and this electric conductivity is to have in the water of ATH of 10wt.% to measure in water.This flame-retarded resin also comprises at least a synthetic resins, and commonly used optional any one or the more additives in this area.
In some embodiments, ATH of the present invention is further characterized in that the soluble soda content that has less than about 0.1wt.%.
In some embodiments, the present invention relates to as above reach ATH particle as described below.
Detailed Description Of The Invention
ATH means aluminium hydroxide and this area various titles that refer to this mineral flame retardants commonly used, for example hydrate of aluminium, aluminum trihydrate, three aluminium hydroxides etc. as used herein.
It should be noted all grain diameter measurement result, i.e. d disclosed herein 10, d 50And d 90, adopt Cilas 1064 L laser spectrum analysers to obtain by laser diffraction measurement from Kang Ta (Quantachrome).Usually can be by at first the sample of suitable water dispersant solution (preparation is referring to following) charging apparatus being prepared to carry out measurement d used herein in the container 10, d 50And d 90Step.Select to be called as the canonical measure of " particle expert (Particle Expert) " then, also select measurement pattern " scope 1 ", select the device inner parameter of the size-grade distribution that is applied to wish then.Should point out in all measuring processes, make sample be subjected to the ultrasonic wave effect about 60 seconds usually during during dispersion reaching measurement.After background is measured, about 75 to about 100mg samples to be analyzed are placed the sampling receptacle that water/dispersant solution is housed and begin measurement.Prepare water/dispersant solution by at first making enriched material from the CAL Polysalt that BASF (BASF) buys by the 500g Calgon that can buy from KMF experimental chemistry (KMF Laborchemie) and 3 liters.With deionized water this solution is assigned to 10 liters.From these 10 liters of initial liquid, take out 100ml and then further be diluted to 10 liters, then this final solution is used as above-mentioned water-dispersant solution with deionized water.
As mentioned above, the present invention relates to comprise the flame-retardant resin formulation of ATH and at least a synthetic resins.Typically, this flame-retardant resin formulation comprises from about ATH of 5 to about 200phr.In preferred embodiments, this flame-retardant resin formulation comprises that ATH arrives in the scope of about 100phr about 15, preferably arrives in the scope of about 75phr about 15, more preferably arrives in the scope of about 55phr about 20.
The ATH that is used for the present invention practice be characterised in that have one or more, preferred two or more and more preferably three kinds or how following feature.ATH of the present invention may have d 10Arrive in about 1.4 mu m ranges about 0.5, preferably arrive in the scope of about 1.0 μ m d about 0.6 50And about 1.2 in the scope of about 3.0 μ m, preferably about 1.3 in the scope of about 2.8 μ m.In other embodiments, ATH of the present invention may have d 50Arrive in the scope of about 2.6 μ m about 1.4.
Another kind in one or more features that ATH of the present invention may have is d 90Arrive in the scope of about 6.0 μ m about 2.2, preferably arrive in the scope of about 5.5 μ m about 2.5.In other embodiments, ATH of the present invention may have d 90Arrive in the scope of about 5.0 μ m about 2.7.
Another kind in one or more features that ATH of the present invention may have is based on ATH, and total sodiun carbomate inventory is less than about 0.2wt.%.In preferred embodiments, if soluble soda content is the feature of ATH of the present invention, total sodiun carbomate inventory is more preferably less than 0.12wt.% less than 0.18wt.%.Can adopt the company from Dr.Bruno Lange GmbH, Dusseldorf (D ü the sseldorf)/flame photometer M7DC of Germany measures total sodiun carbomate inventory of ATH.In the present invention, measure total sodiun carbomate inventory of ATH, at first 1g ATH is added in the quartz glass bowl, in quartz glass bowl, add the 3ml vitriol oil then, and with the glass stick material in the stirred glass bowl carefully.Observe this mixture then, and if the not dissolving fully of ATH crystal, add the other 3ml vitriol oil and mix these materials again.On hot-plate, the bowl heating is evaporated fully until excessive sulfuric acid then.Then the material in the bowl is cooled to about room temperature, and adds any salt in about 50ml deionized water dissolving bowl.Then the material in the bowl is kept at elevated temperatures dissolving until salt in about 20 minutes.Material in the glass bowl is cooled to about 20 ℃ then, transfers in the measuring bottle of 500ml, the deionized water and shaking evenly of packing into then.Analyze solution in the measuring bottle of this 500ml with flame photometer then, obtain total sodiun carbomate inventory of ATH.
Another kind in one or more features that used ATH may have in the practice of the present invention is a thermostability, as described in following table 1.Thermostability refers to emit the burst size of the water of ATH as used herein, and can for example thermogravimetric analysiss of enough several heat analysis methods (" TGA ") directly obtain, in the present invention the thermostability by TGA measurement ATH.Before measuring, in baking oven, under about 105 ℃ the ATH sample drying was removed the moisture on surface in 4 hours.Adopt 70 μ l alumina crucibles (the about 12mg of initial weight) at N then 2(70ml per minute) carries out the TGA measurement with plum Teller-Tuo benefit (Mettler Toledo) down, and heating rate is as follows: 30 ℃ to 150 ℃, and 10 ℃ of per minutes, 150 ℃ to 350 ℃, 1 ℃ of per minute, 350 ℃ to 600 ℃, 10 ℃ of per minutes.The TGA temperature of ATH of the present invention can and be based in this case to be measured under the weightless and 2wt.% weightlessness of ATH 1wt.%, the results are shown in the following table 1 of these measurements:
Figure A20068003864700101
The one or more features of ATH of the present invention also may be selected from i) the Toenol 1140 oil number measured according to ISO787/5 is about 15 in the scope of about 50ml/100g, and/or the specific surface area of ii) measuring according to DIN 66132 (BET) arrives about 8m about 2.0 2In the scope of/g.In preferred embodiments, if the Toenol 1140 oil number is the feature of ATH of the present invention, the Toenol 1140 oil number is preferably in greater than 30 to about 50ml/100g scope, more preferably in about scope of 36 to about 46ml/100g.If BET is the feature of ATH of the present invention, the BET specific surface area preferably from about 2.3 to about 6m 2In the scope of/g, more preferably from about 2.5 to about 4.5m 2In the scope of/g.
The electric conductivity of ATH of the present invention also may be one of feature of ATH used during the present invention puts into practice, if like this, electric conductivity is typically in the scope less than about 200 μ S/cm.Should point out, as described below, the solution that comprises water and about 10wt.%ATH based on solution is carried out all conductivity measurements.Preferably, the electric conductivity of ATH of the present invention is less than about 100 μ S/cm.In other embodiments of the present invention, electric conductivity arrives in the scope of about 45 μ S/cm about 20.Employing is from Wissenschaftlich-Technische-
Figure A20068003864700102
GmbH company, the MultiLab 540 conductivity measurement instrument of Er Haimu Wei (Weilheim)/Germany are measured electric conductivity through the following steps: can be from Ge Sifute experimental technique company (Gesellschaft for Labortechnik mbH), the GFL3015 that Bouguer Cheng De/Germany obtains shakes on the equipment, shakes the 10g sample to be analyzed of in the 100ml Erlenmeyer flask (Erlenmeyer flask) and 90ml deionized water (envrionment temperature) 10 minutes with maximum performance.Then conductive electrode is immersed in this suspension and measure electric conductivity.
In other embodiments, the further feature of ATH of the present invention can be to have the soluble soda content less than about 0.1wt.% based on ATH.In other embodiments, the further feature of ATH of the present invention can be to have based on the ATH soluble soda content and arrive in the scope of about 0.1wt.% greater than about 0.001, in some embodiments, arrive in the scope of about 0.1wt.% about 0.02 based on the ATH soluble soda content.And in other embodiments, the further feature of ATH of the present invention can be to have soluble soda content from about 0.001 in scope less than 0.02wt.%.Measure soluble soda content by flame photometer.In order to measure soluble soda content, following preparation sample solution: with the 20g sample transfer in the 1000ml volumetric flask, and in water-bath about 95 ℃ leached about 45 minutes down with about 250ml deionized water.Then this bottle is cooled to 20 ℃, the deionized water of packing into shakes evenly to calibration mark.After the sample sedimentation, in bottleneck, form limpid solution, then with filtration syringe or flame photometer can be measured required solution amount with separating centrifuge and from this bottle, shift out.
Yet, if described in the present invention practice used ATH only have a feature, this feature is soluble sodiun carbomate inventory so.The inventor is relevant with the sodiun carbomate inventory of ATH in this thermostability of unexpectedly finding ATH.Although it is relevant with total sodiun carbomate inventory of ATH that experimental evidence shows thermostability, do not wish to be bound by theory, the inventor thinks that in this thermostability of ATH raising of the present invention is relevant with the content of soluble soda, based on total soda, this soluble soda typically accounts in about 70 to about 99% the scope of total sodiun carbomate inventory (as mentioned above, comprise preferred embodiment), surplus is solvable soda, and total sodiun carbomate inventory of used ATH typically in the scope less than about 0.18wt.%, is preferably based on ATH based on ATH in the scope less than about 0.12wt.% in the present invention practice.
Flame-retardant resin formulation of the present invention comprises at least a synthetic resins that is selected from Resins, epoxy, novolac resin, phosphorous resin such as DOPO, brominated epoxy resin, unsaturated polyester resin and the vinyl ester, in some cases more than a kind of.
This flame-retardant resin formulation also can contain this area other additive commonly used.The non-limitative example that is applicable to other additive of flame-retardant resin formulation of the present invention comprises other fire retardant based on for example bromine, phosphorus or nitrogen; Solvent, solidifying agent such as stiffening agent or promotor, dispersion agent or phosphorus compound, thin silica, clay or talcum.The ratio of the additive that other is optional is conventional and can changes to adapt to the needs of any given situation.
The component combination of polymer formulators and the preferred method that adds are to adopt high shear mixing.For example, by a mixing tank (head mixer) of for example being made by Sai Duolisi (Silverson) company is sheared.The further processing of resin extender is mixed into " prepreg " stage, make the solidified laminating material then, this is the common situation of this area and description is arranged in the literature, for example Mu Ge is attached to it herein as a reference in full as " Resins, epoxy handbook " (" Handbook of Epoxide Resins ") that-Hull (McGraw-Hill) books company publishes.
More than describe and relate to several embodiments of the present invention.One skilled in the art will realize that in order to realize that purport of the present invention can design same effectively other embodiment.The following example will illustrate the present invention, but and not mean that and be subjected to any type of restriction.
Embodiment
Embodiment 1
In the present embodiment, can be from two kinds of commercially available ATH product Martinal of Martin Si Virco N. V. (Martinswerk GmbH) acquisition
Figure A20068003864700121
OL-104 LE and Martinal The thermostability of OL-104 WE and the thermostability of ATH of the present invention compare.According to TGA experimental measurement thermostability.As shown in Figure 1, ATH rank of the present invention has than the better thermostability of present obtainable product.
Embodiment 2
In order further to analyze thermostability according to ATH of the present invention, prepared preparation of epoxy resin laminates (for the simulate press circuit card), it is used according to ATH of the present invention and fills, and with the commercial trade mark that obtains: Martinal
Figure A20068003864700123
OL-104 LE and OL-104 WE fill.Manufacturing technology by so-called hand laid (HLU) prepares this preparation of epoxy resin laminates, and floating tin test method (solder float test) according to IPC4101 (IPC-TM-650) afterwards, studying thermostability by the stratified time of laminating material of in tin bath, measuring 8 layers in 288+/-5 ℃ down.
Resins is based on 2 kinds of stock mix (stock mixs) as described below.
Stock mix 1
Under the assistance of Sai Duolisi (Silverson) high-speed shearing machine L4R, will be in 450g acetone from 1250g Epikote 1001 resin dissolves of shell chemical company (Shell Chemicals company).Stir after 20 minutes, this solution (" Epikote base resin ") is limpid.Should point out to stop stirring and make temperature reduce about 5 ℃ if temperature surpasses 50 ℃.Continue to stir limpid then until solution becomes.
Except Epikote base resin,, add the 50g Dyhard RU 100 in the dinethylformamide (DMF) and prepare Dyhard RU 100 solution (" dicyandiamide solution " (dicy solution)) by to 450g N.The 2.5g glyoxal ethyline is added in this clear solution, and it is used to finish from the dissolver of Ge Ciman technical process company limited (VMA Getzmanncompany).
This dicyandiamide solution is added in the Epikote base resin, and at room temperature stirred this mixture 10 minutes.Stock mix 1 is placed 24 hours with aging.
Stock mix 2
Stock mix 2 is based on the commercial D.E.N.438 that can obtain from German Dow Chemical (DOW Chemicalscompany).For viscosity that reduces D.E.N.438 and the requirement of measuring 500g, in water-bath, it is heated to from about 80 to about 90 ℃ scope.Afterwards it is cooled to 50 ℃ and be dissolved in the 100g acetone.Adopt Sai Duolisi (Silverson) high-shear mixer L4R to stir this mixture with 30～40% of top speed.
By to 180g N, add 15g Dyhard RU 100 (dicyandiamide) the preparation second Dyhard RU 100 solution (" the second dicyandiamide solution " (second dicy solution)) in the dinethylformamide (DMF).It is limpid until solution to adopt dissolver (from Ge Ciman technical process company limited (VMA Getzmann company)) to stir this solution, adds the 1.0g glyoxal ethyline then.
Add to the second dicyandiamide solution in the D.E.N.438 base resin and at room temperature stirred this mixture 10 minutes.Stock mix 2 is aging standby after 24 hours.
The preparation of preparation of epoxy resin laminates
By with 100g stock mix 1 and 80g stock mix 2 with commercial can be from BYK-Chemie, 1g Byk LP W 20037 dispersion agents that GmbH company obtains are mixed together 1 minute with 30～40% of maximum speed of revolution, the Resins, epoxy that preparation aluminium hydroxide is filled.Then with 50g according to ATH of the present invention or 50gMartinal
Figure A20068003864700131
OL-104/WE or 50g Martinal
Figure A20068003864700132
OL-104/LE mixes with Resins, epoxy, forms three kinds of different ATH/ resin compounds.In Sai Duolisi (Silverson) high-shear mixer, in about 5 minutes time, add ATH once more with 30～40% of maximum speed of revolution.Equally,, stop stirring and make temperature reduce about 5 ℃, continue then to mix about 5 minutes of total mixing time if temperature surpasses 50 ℃.
In order to prepare epoxy laminate material, the ATH/ resin compound of in the wide container of 300mm, packing into.With eight sheet glass cloth (210g/m 2) be cut into the size of 180mm * 250mm, and with an end of every at the top of woven fiber glass and 2 battens of bottom nail (5mm * 10mm * 220mm).The woven fiber glass of preparation is immersed the ATH/ resin compound respectively, and be loaded with resin, additionally be brushed with the ATH/ resin compound, thereby prepare the woven fiber glass of dipping in order to ensure whole woven fiber glass.
The woven fiber glass of dipping is fixed on the experiment table.Remove superfluous resin by two the round metal bars that on the glass cloth surface of dipping, roll.Woven fiber glass in 160 ℃ of dryings 90 seconds, is cooled to room temperature then in baking oven.To between the 42wt.%, it measures by the prepared weight of woven fiber glass before uncoated resin and after coated with resins of weighing the resin of each drying sheet--content at 38wt.%.Woven fiber glass is cut into the size of 150mm * 200mm.Be stacked to 8 layers, and can be from the commercial Tedlar that obtains of Du Pont (Dupont) with 2 layers Add the top and the bottom that are located at the woven fiber glass of cutting.Adopt 195kp/cm down at 170 ℃ 2Pressure press these laminations.Remove Tedlar after being cooled to room temperature
Figure A20068003864700142
Layer.The laminating material that gained is 8 layers has from about 38 resin contents in about 42wt.% scope, and the thickness of 0.8mm.
Then each cloth of 8 layers is cut into the part of detecting of 9 40mm * 50mm.Measure the separation time of each part of detecting in the following way, study the thermostability of these 8 layers of preparation of epoxy resin laminates.Test article is fixed on the fixer of the divalence tin bath that immerses 288+/-5 ℃.Measuring Time is until producing layering first.Detect layering by impact, and be confirmed by visual inspection to fixer.By the aluminium hydroxide thermal endothermic decomposition is that aluminum oxide and water cause layering.According to above-mentioned steps preparation and not the preparation of epoxy resin laminates of aluminium hydroxide after 10 minutes, do not show layering.
Fig. 2 explanation contains with good grounds ATH of the present invention as the part of detecting of filler stratified relative mean time, and contains Martinal
Figure A20068003864700143
OL-104/WE and Martinal
Figure A20068003864700144
The part of detecting of OL-104/LE is compared,, the latter is reached be set at 100% stratified mean time thus.The separation time of listing is based on a kind of 8 layers mean value of 9 test article of preparation of epoxy resin laminates.Shown respectively result according to 2 kinds of laminating materials of above-mentioned steps preparation.
As shown in Figure 2, as by reach measure stratified mean time, adopt ATH particle of the present invention to show and be better than containing the thermostability of conventional ATH as those resins of filler as the preparation of epoxy resin laminates of filler.

Claims (42)

1. flame-retardant resin formulation comprises:
A) has aluminium hydroxide (" the ATH ") particle of at least a or how following feature: i) d 10From about 0.5 in the scope of about 1.4 μ m; Ii) d 50From about 1.2 in the scope of about 3.0 μ m; Iii) d 90From about 2.2 in the scope of about 6.0 μ m; Iii) based on ATH, total sodiun carbomate inventory is less than about 0.2wt.%;
Iv) the Toenol 1140 oil number is in about scope of 15 to about 50ml/100g; And v) the BET specific surface area from about 2.0 to about 8m 2In the scope of/g; And
B) at least a synthetic resins,
Wherein, the electric conductivity of ATH is less than about 200 μ S/cm.
2. according to the flame-retardant resin formulation of claim 1, wherein, described ATH has the soluble soda content less than about 0.1wt.%.
3. according to the flame-retardant resin formulation of claim 2, wherein, described ATH has i) d 10From about 0.6 in the scope of about 1.0 μ m; And/or ii) d 50From about 1.3 in the scope of about 2.8 μ m or d 50From about 1.4 in the scope of about 2.6 μ m; And/or iii) d 90From about 2.5 in the scope of about 5.5 μ m or d 90From about 2.7 in the scope of about 5.0 μ m.
4. according to the flame-retardant resin formulation of claim 3, wherein, described ATH has the total sodiun carbomate inventory less than 0.18wt.%.
5. according to the flame-retardant resin formulation of claim 3, wherein, described ATH has the total sodiun carbomate inventory less than 0.12wt.% based on ATH.
6. according to each flame-retardant resin formulation in the claim 3～5, wherein, described ATH has TGA and is distributed as:
1wt.％TGA(℃) 2wt.％TGA(℃) 210～225 220～235
Perhaps
1wt.％TGA(℃) 2wt.％TGA(℃) 210～220 220～230
Perhaps
1wt.％TGA(℃) 2wt.％TGA(℃) 214～218 224～228
。
7. according to the flame-retardant resin formulation of claim 6, wherein, described ATH has from greater than 30 Toenol 1140 oil numbers in about 50ml/100g scope.
8. according to the flame-retardant resin formulation of claim 7, wherein, described ATH has from about 2.3 to about 6m 2BET specific surface area in the/g scope.
9. according to each flame-retardant resin formulation in claim 4 or 5, wherein, described ATH has based on ATH from about 0.001 soluble soda content in about 0.1wt.% scope.
10. according to each flame-retardant resin formulation in claim 4 or 5, wherein, described ATH have from about 0.001 to less than the soluble soda content in the scope of 0.02wt.%.
11. according to the flame-retardant resin formulation of claim 9, wherein, based on total sodiun carbomate inventory, the soluble sodiun carbomate inventory of described ATH arrives in the scope of about 99wt.% at about 70 of total sodiun carbomate inventory.
12. according to the flame-retardant resin formulation of claim 11, wherein, described ATH has the electric conductivity less than about 100 μ S/cm.
13. according to the flame-retardant resin formulation of claim 10, wherein, described ATH has from about 20 electric conductivitys in about 45 μ S/cm scopes.
14. a flame-retardant resin formulation comprises:
A) has the aluminium hydroxide (" ATH ") of at least a or how following feature: i) d 10From about 0.6 in the scope of about 1.0 μ m; Ii) d 50From about 1.3 in the scope of about 2.6 μ m; Iii) d 90From about 2.7 in the scope of about 5.0 μ m; Iii) based on ATH, total sodiun carbomate inventory is less than about 0.12wt.%; Iv) the Toenol 1140 oil number is in about scope of 15 to about 50ml/100g; And v) the BET specific surface area from about 2.0 to about 6m 2In the scope of/g; And
B) at least a synthetic resins,
Wherein, at least a synthetic resins is selected from Resins, epoxy, novolac resin, phosphorous resin, brominated epoxy resin, unsaturated polyester resin and vinyl ester, the electric conductivity of ATH is less than about 100 μ S/cm, described ATH has the soluble soda content less than about 0.1wt.%, and TGA is distributed as:
1wt.％TGA(℃) 2wt.％TGA(℃) 210～225 220～235
。
15. according to the flame-retardant resin formulation of claim 14, wherein, described ATH has TGA and is distributed as:
1wt.％TGA(℃) 2wt.％TGA(℃) 210～220 220～230
Perhaps
1wt.％TGA(℃) 2wt.％TGA(℃) 214～218 224～228
。
16. according to the flame-retardant resin formulation of claim 15, wherein, described ATH has from greater than the Toenol 1140 oil number in 30 to about 50ml/100g the scope.
17. according to the flame-retardant polymer formulation of claim 16, wherein, described ATH have from about 2.5 to about 4.5m 2BET specific surface area in the scope of/g.
18. according to each flame-retardant resin formulation in claim 15 or 17, wherein, described ATH has based on ATH in the soluble soda content in about scope of 0.001 to about 0.1wt.%.
19. according to each flame-retardant resin formulation in claim 15 or 17, wherein, described ATH have from about 0.001 to less than the soluble soda content in the scope of 0.02wt.%.
20. according to the flame-retardant resin formulation of claim 19, wherein, based on total sodiun carbomate inventory, the soluble sodiun carbomate inventory of described ATH arrives in the scope of about 99wt.% at about 70 of total sodiun carbomate inventory.
21. according to the flame-retardant resin formulation of claim 19, wherein, described ATH has from about 20 electric conductivitys in about 45 μ S/cm scopes.
22. the epoxy laminate material of making by the flame-retardant resin formulation of claim 21.
23. the epoxy laminate material of making by the flame-retardant resin formulation of claim 14.
24.ATH, have: from about 0.6 d in about 1.0 mu m ranges 10From about 1.2 d in about 3.0 mu m ranges 50From about 2.5 d in about 6.0 mu m ranges 90Based on ATH, less than total sodiun carbomate inventory of about 0.2wt.%, the Toenol 1140 oil number of measuring according to ISO 787-5:1980 is in about scope of 15 to about 40ml/100g; And the specific surface area of measuring according to DIN-66132 (BET) from about 2.0 to about 5m 2In the scope of/g, wherein, the electric conductivity of ATH is less than about 200 μ S/cm, and this electric conductivity is to have in the water of ATH of 10wt.% to measure in water.
25. according to the ATH of claim 24, wherein, described ATH has the soluble soda content less than about 0.1wt.%.
26. according to the ATH of claim 25, wherein, described ATH has from about 0.6 d in about 1.0 mu m ranges 10
27. according to the ATH of claim 26, wherein, described ATH has from about 1.3 d in about 2.8 mu m ranges 50
28. according to the ATH of claim 25, wherein, described ATH has from about 1.4 d in about 2.6 mu m ranges 50
29. according to the ATH of claim 27, wherein, described ATH has from about 2.5 d in about 5.5 mu m ranges 90
30. according to the ATH of claim 28, wherein, described ATH has from about 2.7 d in about 5.0 mu m ranges 90
31. according to the ATH of claim 29, wherein, described ATH has the total sodiun carbomate inventory less than about 0.18wt.%.
32. according to the ATH of claim 30, wherein, described ATH has the total sodiun carbomate inventory less than about 0.12wt.% based on ATH.
33. according to the ATH of claim 25, wherein, described ATH has the thermostability of being measured by thermogravimetric analysis (TGA) and is:
1wt.％TGA(℃) 2wt.％TGA(℃) 210～225 220～235
。
34. according to the ATH of claim 31, wherein, described ATH has the thermostability of being measured by thermogravimetric analysis (TGA) and is:
1wt.％TGA(℃) 2wt.％TGA(℃) 210～220 220～230
。
35. according to the ATH of claim 32, wherein, described ATH has the thermostability of being measured by thermogravimetric analysis (TGA) and is:
1wt.％TGA(℃) 2wt.％TGA(℃) 214～218 224～228
。
36. according to the ATH of claim 34, wherein, described ATH has from greater than about 30 Toenol 1140 oil numbers in about 40ml/100g scope.
37. according to the ATH of claim 36, wherein, described ATH have from about 2.3 to about 4.3m 2BET specific surface area in the scope of/g.
38. according to the ATH of claim 34, wherein, described ATH has the electric conductivity less than about 100 μ S/cm, this electric conductivity is to have in the water of ATH of 10wt.% to measure in water.
39. according to the ATH of claim 35, wherein, described ATH has about 20 electric conductivitys in about 45 μ S/cm scopes, this electric conductivity is to have in the water of ATH of 10wt.% to measure in water.
40. according to the ATH of claim 38, wherein, described ATH has based on ATH from greater than about 0.02 soluble soda content in about 0.1wt.% scope.
41. according to the ATH of claim 38, wherein, described ATH has less than the soluble soda content in the 0.02wt.% scope.
42. according to the ATH of claim 25, wherein, based on total soda, the soluble sodiun carbomate inventory of described ATH arrives in the scope of about 99wt.% at about 70 of total sodiun carbomate inventory.
CNA2006800386477A 2005-10-18 2006-10-12 Thermally stable aluminum hydroxide particles and their use as fillers in epoxy laminate resins Pending CN101291878A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110088183A (en) * 2016-12-13 2019-08-02 纳幕尔杜邦公司 The durable surface treatment of solid polymer height

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110088183A (en) * 2016-12-13 2019-08-02 纳幕尔杜邦公司 The durable surface treatment of solid polymer height

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