CN1667029A - Process for preparing magnesium hydroxide loose nano blocked flame retardant and products therefrom - Google Patents
Process for preparing magnesium hydroxide loose nano blocked flame retardant and products therefrom Download PDFInfo
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- CN1667029A CN1667029A CN 200510033253 CN200510033253A CN1667029A CN 1667029 A CN1667029 A CN 1667029A CN 200510033253 CN200510033253 CN 200510033253 CN 200510033253 A CN200510033253 A CN 200510033253A CN 1667029 A CN1667029 A CN 1667029A
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- magnesium hydroxide
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- flame retardant
- nano particle
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 62
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 62
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 62
- 239000003063 flame retardant Substances 0.000 title claims abstract description 43
- 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 claims description 35
- 238000004519 manufacturing process Methods 0.000 title abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000003607 modifier Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 5
- 239000000194 fatty acid Substances 0.000 claims abstract description 5
- 229930195729 fatty acid Natural products 0.000 claims abstract description 5
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000011777 magnesium Substances 0.000 claims abstract description 4
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 4
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 claims abstract description 4
- 239000002105 nanoparticle Substances 0.000 claims description 42
- 239000002088 nanocapsule Substances 0.000 claims description 11
- 238000011049 filling Methods 0.000 claims description 8
- 239000011148 porous material Substances 0.000 claims description 6
- 239000000779 smoke Substances 0.000 claims description 6
- 238000005273 aeration Methods 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 238000004945 emulsification Methods 0.000 claims description 5
- 238000000265 homogenisation Methods 0.000 claims description 5
- 238000011065 in-situ storage Methods 0.000 claims description 5
- 239000002861 polymer material Substances 0.000 claims description 5
- -1 silicate ester Chemical class 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 2
- 230000009471 action Effects 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 239000002563 ionic surfactant Substances 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 239000002736 nonionic surfactant Substances 0.000 claims description 2
- 229920000620 organic polymer Polymers 0.000 claims description 2
- 230000000979 retarding effect Effects 0.000 claims description 2
- 235000002639 sodium chloride Nutrition 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 abstract description 2
- 239000000920 calcium hydroxide Substances 0.000 abstract description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 abstract description 2
- 235000011116 calcium hydroxide Nutrition 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000002775 capsule Substances 0.000 abstract 1
- 230000008569 process Effects 0.000 description 12
- 229920000459 Nitrile rubber Polymers 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 239000011858 nanopowder Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 239000004636 vulcanized rubber Substances 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 229920002292 Nylon 6 Polymers 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000012796 inorganic flame retardant Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910015853 MSO4 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 241000276425 Xiphophorus maculatus Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 230000009972 noncorrosive effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Fireproofing Substances (AREA)
Abstract
This invention relates to manufacturing method and product of magnesium hydroxide loosen nanometer particle block fire retardant, it belongs to unorganic chemical nanometer material manufacturing. The capability of nanometer particle surface adsorbability is used. During the preparation process, after it is coated by surface modifier, high speed exiguous air current bubble is added, and it is strongly gas charged, dispersed, isotroped and emulsified in order to make massive gas between the created nanometer capsule particles and form multi material, then magnesium hydroxide loosen nanometer particle block fire retardant is made. The equipment of this invention is simple, technique is fluency, and can be executed scale generation. In bubble cap disc style agitator, material is water soluble salt or oxide of magnesium, precipitant is NH3.H2O, NaOH or Ca(OH)2, surface modifier is at least one of fatty acid, poly unsaturated fatty acid and its salt, then magnesium hydroxide loosen nanometer particle block fire retardant is made after it is separated and purified. The magnesium hydroxide particle scale consisted has at least one dimension in 1-100nm extent in three space.
Description
[ technical field]A method for producing a semiconductor device
The invention relates to a method for preparing magnesium hydroxide loose nano particle block fire retardant and a product thereof, belonging to the inorganic chemical industry nano material manufacturing industry.
[ background of the invention]
The inorganic material magnesium hydroxide is an additive flame retardant of a high polymer material, and compared with the similar inorganic flame retardants, the magnesium hydroxide has the advantages that: the magnesium hydroxide has triple functions of flame retardance, smoke abatement and filling, and endows the material with smoke-free and non-corrosive properties, and can obtain better flame retardance and smoke abatement effects; the magnesium hydroxide has no harmful substance emission in the production, use and waste processes, and does not cause environmental pollution; the initial thermal decomposition temperature of the magnesium hydroxide is 340 ℃ to 490 ℃ and the decomposition is complete and is 140 ℃ higher than the decomposition temperature of the aluminum hydroxide. Its total endotherm is 44.8KJ/mol, which is about 17% higher than the total endotherm of aluminum hydroxide. Therefore, the high-temperature-resistant and high-temperature-resistant composite material can bear higher processing temperature, is favorable for accelerating extrusion molding speed in product production and shortening molding time; the magnesium hydroxide can promote the carbon formation of the polymer to form a protective layer and exert better flame retardant effect besides self dehydration during combustion and decomposition; and (V) the magnesium hydroxide is matched with other flame retardants to show good flame-retardant synergistic effect. Therefore, in recent years, magnesium hydroxide has been highly regarded as a flame retardant and has been rapidly developed. At home and abroad, the magnesium hydroxide is consistently considered to be the main inorganic flame retardant, and the application of the magnesium hydroxide is one of important directions for the development of the flame retardant. However, since the particles of the common magnesium hydroxide flame retardant have strong agglomeration tendency and are not easy to disperse, the molecules have strong polarity, and the dispersibility and compatibility in the high polymer material are poor, the mechanical property of the flame retardant material is sharply reduced. Currently, the method for solving the problem is to refine magnesium hydroxide particles to prepare fine powder, submicron powder or nano powder. The magnesium hydroxide nano powder has better flame retardant and smoke abatement effects than fine powder and submicron powder, and particularly has better filling enhancement effect, thus being the development direction. However, the nano powder has certain problems, such as the high surface energy of the nano powder makes the nano particles easy to agglomerate. The common magnesium hydroxide nano powder is fine compact nano particle powder formed by agglomeration of a plurality of nano particles. The compact nano particle powder is difficult to disperse in a high polymer material, and the mechanical strength of the flame retardant material can still be reduced. Meanwhile, in the process of preparing the compact nano particle powder, the problems of difficult filtration, difficult washing and difficult drying are caused, and a plurality of troubles in the process are caused. And the fine powder is easy to fly and cause environmental pollution.The invention provides a new process for preparing a nano magnesium hydroxide flame retardant material by three people of inventor Song Fang Hua and the like at the university of Beijing chemical industry in China, and the invention patent in China is obtained, wherein the publication number is CN1128199C, the publication number is 11/19/2003 and the patent number is 01141787.0, and the main content of the process is that a refined magnesium chloride solution obtained from old brine or magnesite and industrial ammonia water or ammonia gas are used as raw materials, and a supergravity (rotating packed bed) technology is adopted to prepare the nano magnesium hydroxide flame retardant by using a liquid-liquid phase reaction or a liquid-gas phase reaction mode. The process provided by the invention overcomes the defects of complexity, high cost, uneven particle size, difficulty in control and the like of the traditional process. However, the process of the invention has certain weaknesses after careful analysis: the added equipment cost is high, the technological process and the obtained product are not satisfactory, and improvement is still needed. Aiming at the defects of the traditional process and the process, the invention provides a more reasonable preparation method, and the product is a loose nano particle block.
[ summary of the invention]
The invention aims to provide a method for preparing a magnesium hydroxide loose type nano particle block flame retardant and a product thereof, which utilize the property of absorbing a large amount of gas on the surface of nano particles, in the process of preparing the magnesium hydroxide loose type nano particles, after the nano particles are coated by a surface modifier, high-speed micro bubble flow is introduced, and the nano particles are strongly aerated, dispersed, homogenized and emulsified, so that a large amount of gas is absorbed on the surfaces of the generated magnesium hydroxide nano capsule particles, the gas filled among the nano capsule particles becomes loose, a porous material is formed, and the magnesium hydroxide loose type nano particle block flame retardant is prepared by filtering, washing and drying. The steps taken to implement the invention are as follows:
firstly, raw materials:
1. water soluble salt or oxide of magnesium as raw material
The general molecular formula is as follows: MCL2、MSO4MO, M is metal magnesium
The producing area: purchased from Guangzhou
2. Settling agent
(1) Aqueous ammonia
The molecular formula is as follows: NH (NH)3·H2O
The producing area: purchased from Guangzhou
(2) Sodium hydroxide
The molecular formula is as follows: NaOH
The producing area: purchased from Guangzhou
(3) Calcium hydroxide
The molecular formula is as follows: ca (OH)2
The producing area: provided by applied chemistry research institute of Zhongshan City
II, surface modifier
1. Fatty acids
The general molecular formula is as follows: RCOOH R is a hydrocarbyl radical
The producing area: purchased from Zhongshan City
2. Polyunsaturated fatty acids
The general molecular formula is as follows:
r is hydrocarbyl-
The producing area: purchased from Zhongshan City
3. Silicates, i.e. alkoxysilanes
The general molecular formula is as follows: si (OR)4R is alkyl
The producing area: purchased from Zhongshan City
4. Titanates, i.e. titanate coupling agents
The general molecular formula is as follows: ti (OR)4R is alkyl
The producing area: purchased from Zhongshan City
Third, chemical reaction equation:
reaction equipment, steps and mechanism
Reaction equipment:
the name and the model number are as follows: NA-1 series, bubble cap disc type agitator reactor
The producing area: developed by applied chemistry research institute of Zhongshan City
(II) reaction steps and mechanism:
1. in a bubble-cap disc-type stirred reactor at a temperature of 15-80 ℃ with magnesiumUsing water-soluble salt or oxide as raw material and NH3·H2O, NaOH or Ca (OH)2The sedimentation agent is a high-speed bubble flow generated by a stirrer, and the high-speed bubble flow is subjected to strong aeration, dispersion, homogenization and emulsification, and the reaction time is 30-90 minutes to generate magnesium hydroxide nano particles;
2. simultaneously, at least one of fatty acid, polyunsaturated fatty acid and salt thereof, silicate ester, titanate or ionic and nonionic surfactants is selected as a surface modifier, and in-situ coating is carried out to generate magnesium hydroxide nano-capsule particles;
3. under the action of powerful aeration, dispersion, homogenization and emulsification of high-speed fine bubble flow, a large amount of gas is filled among the nano capsule particles to become loose, so that a porous material is formed, and then the porous material is filtered, washed and dried to prepare the magnesium hydroxide loose nano particle block flame retardant.
4. The magnesium hydroxide loose nano particle block is a loose block in appearance, the size of the magnesium hydroxide particles is formed, and at least one dimension of the magnesium hydroxide loose nano particle block in a three-dimensional space is within the range of 1-100 nm.
5. In actual production, magnesium ions in the bulk magnesium hydroxide loose nanoparticle block are partially replaced by other metal ions (such as aluminum ions), and hydroxide radicals are partially replaced by other negative ions (such as carbonate) to form the composite hydroxide nanoparticle block flame retardant.
6. Experiments prove that the magnesium hydroxide loose nano particle block has obvious flame retardant, smoke abatement and filling enhancement functions on organic polymer materials.
From the above, we can understand the advantages of the present invention as follows:
the bubble cap disc type stirrer with powerful aerating, dispersing, homogenizing and emulsifying functions is adopted to aerate a large amount of magnesium hydroxide nano capsule particles to manufacture loose nano particle blocks, so that the filtering, washing and drying processes are simple and easy to implement, the equipment is simple, and the manufacturing cost is low; secondly, because the surface modifier is added in the reaction process and the coating is carried out in situ, the process becomes smoother;
compared with the common compact nano powder, the loose nano particle block does not fly, does not pollute the environment and can implement large-scale production; the product has excellent flame retarding, smoke eliminating and stuffing strengthening functions.
[ description of the drawings]
The manufacturing process and product of the present invention are further illustrated by the following description and specific embodiments in conjunction with the accompanying drawings.
FIG. 1 is a flow chart of the method for preparing the magnesium hydroxide loose nano particle block flame retardant.
[ detailed description]according to the present embodiment
Example 1
Dissolving magnesium chloride (10mol) in water in a reactor with a bubble disk type stirrer (patent application number: 200420044185.8), adding ammonia water (25-28%, 2000ml), fully stirring for reaction, adding a fatty acid surface modifier, coating in situ, utilizing high-speed fine bubble flow generated by the bubble disk type stirrer, strongly aerating, dispersing, homogenizing and emulsifying to enable generated magnesium hydroxide nanocapsule particles to fully adsorb gas or the nanocapsule particles to be adsorbed on the surfaces of bubbles, filling a large amount of gas among the nanocapsule particles to be loosened to form a porous material, and filtering, washing and drying to prepare the magnesium hydroxide loose type nano particle block flame retardant. The prepared magnesium hydroxide loose type nano particle block flame retardant is detected by a scanning electron microscope, the magnesium hydroxide nano particles are platy, the thickness is less than 50nm, and the nano particles with the length less than 180nm account for more than 85 percent. Through mixing, the flame retardant can be dispersed into Nitrile Butadiene Rubber (NBR) vulcanized rubber, and the functions of the flame retardant nano-materials are obviously shown. When the addition amount of the flame retardant is 100% of the vulcanized nitrile rubber, the data of the influence of the magnesium hydroxide loose type nano particle block flame retardant on the performances of the vulcanized nitrile rubber are shown in the table 1.
Table 1. influence of magnesium hydroxide loose type nano particle block flame retardant on the performance of nitrile rubber vulcanized rubber.
| Item | Detecting data | Change in Property% | |
| NBR | 100 | 100 | / |
| Flame retardant | 0 | 100 | / |
| 100% stress at definite elongation/MPa | 1.34 | 1.88 | 40.3 |
| Tensile strength/MPa | 3.28 | 9.05 | 175.9 |
| Elongation at break/%) | 315 | 630 | 100 |
| Tear Strength/KN/m | 12.32 | 22.37 | 81.6 |
| Shore A hardness/degree | 48 | 63 | 31.3 |
| Oxygen index/% | 18.5 | 27.0 | 45.9 |
When the amount of the flame retardant is 100 parts, the oxygen index of the flame-retardant nitrile rubber vulcanized rubber is increased to 27.0 from 18.5 of pure nitrile rubber, the tensile strength, the elongation at break and the tearing strength are increased to 1.88Mpa, 630 percent and 22.37KN/m from 1.34Mpa, 315 percent and 12.32KN/m respectively, the flame retardance and the mechanical property are greatly increased, which shows that the magnesium hydroxide loose type nano particles are uniformly dispersed in the nitrile rubber vulcanized rubber, the flame retardant property and the reinforced filling property are excellent, and the nano function of the flame retardant is fully shown.
Example 2
In a reactor with a bubble cap disc type stirrer, magnesium chloride solution (10mol) with certain concentration determined by measurement reacts with NaOH (containing NaOH15mol) with certain concentration, surfactant isadded, in-situ coating is carried out, high-speed fine bubble flow generated by the bubble cap disc type stirrer is utilized, strong aeration, dispersion, homogenization and emulsification are carried out, so that the generated magnesium hydroxide nano capsule particles form loose porous materials, and the loose type nano particle block flame retardant of magnesium hydroxide is prepared after filtration, washing and drying. The X-ray diffraction pattern of the prepared magnesium hydroxide loose nanoparticle block flame retardant is 17.8 degrees, 37.5 degrees, 50.1 degrees and 58.1 degrees at 2 theta, and typical diffraction peaks of magnesium hydroxide crystals appear. The particle size of 90.18mm is 89.5% as detected by Malvern particle size analyzer. When the nano magnesium hydroxide is added into nylon 6 resin, and the addition amount is 30%, the tensile strength is increased from 45MPa of pure nylon 6 to 76MPa, and the excellent reinforcing filling effect is shown. When the nano magnesium hydroxide and the red phosphorus are used together, the flame retardant property of the nylon 6 composite material reaches V-0 grade when the dosage of the magnesium hydroxide and the red phosphorus is respectively 30phr and 20 phr.
Claims (3)
1. The loose magnesium hydroxide nano particle block fire retardant is prepared with water soluble salt or oxide of magnesium as material and NH3·H2O, NaOH or Ca (OH)2Is a settling agent and is characterized in that:
reacting in a reactor capable of generating high-speed bubble flow and performing powerful aeration, dispersion, homogenization and emulsification to generate magnesium hydroxide nano particles;
(II) at least one of fatty acid, polyunsaturated fatty acid and salt thereof, silicate ester, titanate or ionic and nonionic surfactant is used as a surface modifier for in-situ coating to generate magnesium hydroxide nano capsule particles;
(III) under the action of powerful aeration, dispersion, homogenization and emulsification of high-speed fine bubble flow, filling a large amount of gas into the nano capsule particles to loosen and form a porous material, and then separating and purifying the expected product to prepare the magnesium hydroxide loose nano particle block flame retardant;
and (IV) the magnesium hydroxide loose nano particle block is loose, has the appearance of a loose block, and consists of the dimension of magnesium hydroxide particles, and at least one dimension of the magnesium hydroxide loose nano particle block in a three-dimensional space is within the range of 1-100 nm.
2. The method and product for preparing bulk magnesium hydroxide nanoparticle flame retardant according to claim 1, wherein the magnesium ions in the bulk magnesium hydroxide nanoparticles are partially substituted by other metal ions (e.g. aluminum ions) and the hydroxide groups are partially substituted by other negative ions (e.g. carbonate).
3. The method for preparing magnesium hydroxide loose nano particle block fire retardant and the product thereof according to claim 1, wherein the magnesium hydroxide loose nano particle block has the functions of fire retarding, smoke abatement and enhanced filling for organic polymer materials.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510033253XA CN1295270C (en) | 2005-02-23 | 2005-02-23 | Process for preparing magnesium hydroxide loose nano blocked flame retardant and products therefrom |
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| CNB200510033253XA CN1295270C (en) | 2005-02-23 | 2005-02-23 | Process for preparing magnesium hydroxide loose nano blocked flame retardant and products therefrom |
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| CN1667029A true CN1667029A (en) | 2005-09-14 |
| CN1295270C CN1295270C (en) | 2007-01-17 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182052B (en) * | 2007-11-16 | 2012-07-18 | 曾能 | Treatment of alkaline black liquor by bubble liquid membrane bittern method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1359853A (en) * | 2000-12-19 | 2002-07-24 | 中国科学技术大学 | Acidular or flaky nano magnesium hydroxide and its preparing process |
| CN1142098C (en) * | 2000-12-28 | 2004-03-17 | 北京化工大学 | Prepn of nanometer-sized magnesium hydroxide |
| CN1128199C (en) * | 2001-09-19 | 2003-11-19 | 北京化工大学 | Preparation process of magnesium hydroxide fire-retarding nanomaterial |
| CN1255321C (en) * | 2002-12-31 | 2006-05-10 | 浙江大学 | Preparation method of nano-level magnesium hydroxide |
| CN1241977C (en) * | 2003-11-04 | 2006-02-15 | 上海大学 | Method for manufacturing nanometer magnesium hydroxide fire retardant |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101182052B (en) * | 2007-11-16 | 2012-07-18 | 曾能 | Treatment of alkaline black liquor by bubble liquid membrane bittern method |
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| CN1295270C (en) | 2007-01-17 |
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