CN105271336A - Preparation method of high-dispersion superfine aluminium hydroxide - Google Patents
Preparation method of high-dispersion superfine aluminium hydroxide Download PDFInfo
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- CN105271336A CN105271336A CN201510817320.0A CN201510817320A CN105271336A CN 105271336 A CN105271336 A CN 105271336A CN 201510817320 A CN201510817320 A CN 201510817320A CN 105271336 A CN105271336 A CN 105271336A
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Abstract
The invention provides a preparation method of high-dispersion superfine aluminium hydroxide. Superfine aluminium hydroxide is finally obtained by adding seed crystals and dispersion modifier at the same time at a certain reaction temperature with a sodium metaaluminate solution as the raw material, conducting stirring for a certain period of time, and conducting solid-liquid separation, washing, drying and dispersing on obtained pulp, wherein D50 is equal to 0.8-2 micrometers, and D100 is smaller than 10 micrometers. By means of the method, agglomeration of superfine aluminium hydroxide powder is effectively reduced, aggregate in finished products is reduced, the processing performance of high-dispersion superfine aluminium hydroxide is effectively improved, and the high-dispersion superfine aluminium hydroxide can be used for inflaming retarding or filling of wires, cables, rubber, plastic, papermaking, electric insulation and the like.
Description
Technical field
The present invention relates to a kind of preparation method of high-dispersion ultrafine aluminium hydroxide, can be used for electric wire, rubber, plastics, papermaking, electrical insulations etc. fire-retardant or fill.
Background technology
Ultrafine aluminium hydroxide due to its particle superfine, have fire-retardant, eliminate smoke, fill three zones, the industries such as electrician, electronics, electric wire, plastics, rubber are widely used in as high-grade flame retardant filler, except having flame retardancy and smoke suppression effect, the tracking-resistant of product, resistance to electric arc, wear resisting property are all significantly increased.
Because powder granularity is thinner, its specific surface is larger, is therefore easy to reunite, form coacervate, and coacervate its structure in the application course of processing of powder is not easily destroyed, cause filling or spike uneven, product application degradation, makes its quality product class step-down; Limit the add-on of ultrafine aluminium hydroxide differential simultaneously.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of preparation method of high-dispersion ultrafine aluminium hydroxide.Can be used for electric wire, rubber, plastics, papermaking, electrical insulations etc. fire-retardant or fill.
The technical solution adopted in the present invention is: a kind of preparation method of high-dispersion ultrafine aluminium hydroxide, take sodium aluminate solution as raw material, under certain temperature of reaction, dispersed modifier is added while adding crystal seed, after stirring certain hour, the slurries of gained are carried out solid-liquid separation, washing, oven dry and dispersion, finally obtains ultrafine powder aluminium hydroxide, its D
50=0.8 ~ 2um, D
100< 10um.
Concrete steps are, a kind of preparation method of high-dispersion ultrafine aluminium hydroxide, with 100 parts of alumina contents be 220g/L ~ 260g/L, the solution Crater corrosion sodium aluminate solution that is α K=1.4 ~ 1.6 is for raw material, under the temperature of reaction of 55 ~ 75 DEG C, add 0.5 ~ 2 part of crystal seed, add 0.5 ~ 2.0 part of dispersed modifier simultaneously, after stirring reaction 6 ~ 11h, the slurries of gained are carried out solid-liquid separation, washing, oven dry and impact grinding break up, finally obtain ultrafine powder aluminium hydroxide, its D50=0.8 ~ 2um, D100 < 10um.
Described crystal seed is wet milling process aluminium hydroxide seed, seed particle size D
100< 5 μm;
Described dispersed modifier is Trisodium Citrate, silane A-151, amine hydroxybenzene, dispersion agent (AB8030) wherein one or more.
When described impact grinding is broken up, impact grinding main frame frequency is 30 ~ 50HZ, and grading machine frequency is 25 ~ 45HZ.
Compared with prior art, emphasis of the present invention is start with from the principle of powder reuniting, suitable properties-correcting agent is added add crystal seed in building-up process while, while crystal induction aluminum hydroxide crystals heterogeneous nucleation, utilize the dispersant molecule surface-area that compares larger, there is the advantage of hydrophilic/lipophilic amphiprotic group, by the hydroxy combining of the aluminium hydroxide molecule of the effect of hydrogen bond and the little of formation, effective polarity reducing the fine crystals surface generated, surface tension and surface with electricity, fundamentally solve the problem of the hard aggregation of small-crystalline, achieve small particle size product and there is high dispersive performance, in addition, equipment (impact grinding) operating frequency is adjusted in the drying course in products production later stage, solve the soft-agglomerated problem of ultrafine aluminium hydroxide product further, so, in sum, the technology of the present invention chemically with physics two aspect acting in conjunction, effectively reduce the reunion of ultra fine aluminium hydroxide body, decrease the coacervate in finished product, effectively improve its processing characteristics, greatly improve and widen the Application Areas of ultra fine aluminium hydroxide body.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of preparation method of the present invention.
Fig. 2-5 is respectively scanning electron microscope (SEM) photo of embodiment of the present invention 1-4 product.
Embodiment
Below in conjunction with accompanying drawing, method of the present invention is described further.
Embodiment 1
A kind of preparation method of high-dispersion ultrafine aluminium hydroxide, with 100 parts of alumina contents be 235g/L, the solution Crater corrosion sodium aluminate solution that is α K=1.52 is for raw material, under the temperature of reaction of 65 DEG C, 1.2 parts of Trisodium Citrates are added while adding the crystal seed of 1.5 parts of wet grindings, after stirring reaction 8h, the slurries of gained are carried out solid-liquid separation, washing, oven dry and impact grinding break up, impact grinding main frame frequency is 40HZ, grading machine frequency is 35HZ, finally obtain ultrafine powder aluminium hydroxide to pack, product cut size D
100for 7um, accompanying drawing 2 is shown in by product SEM photo.
Embodiment 2
A kind of preparation method of high-dispersion ultrafine aluminium hydroxide, with 100 parts of alumina contents be 220g/L, the solution Crater corrosion sodium aluminate solution that is α K=1.60 is for raw material, under the temperature of reaction of 75 DEG C, 2 parts of amine hydroxybenzenes are added while adding the crystal seed of 2 parts of wet grindings, after stirring reaction 10h, the slurries of gained are carried out solid-liquid separation, washing, oven dry and impact grinding break up, impact grinding main frame frequency is 30HZ, grading machine frequency is 25HZ, finally obtain ultrafine powder aluminium hydroxide to pack, product cut size D
100for 8.5um, accompanying drawing 3 is shown in by product SEM photo.
Embodiment 3
A kind of preparation method of high-dispersion ultrafine aluminium hydroxide, with 100 parts of alumina contents be 260g/L, the solution Crater corrosion sodium aluminate solution that is α K=1.42 is for raw material, under the temperature of reaction of 55 DEG C, 1.2 parts of silane A151 are added while adding the crystal seed of 0.75 part of wet grinding, after stirring reaction 11h, the slurries of gained are carried out solid-liquid separation, washing, oven dry and impact grinding break up, impact grinding main frame frequency is 50HZ, grading machine frequency is 45HZ, finally obtain ultrafine powder aluminium hydroxide to pack, product cut size D
100for 6.5um, accompanying drawing 4 is shown in by product SEM photo.
Embodiment 4
A kind of preparation method of high-dispersion ultrafine aluminium hydroxide, with 100 parts of alumina contents be 245g/L, the solution Crater corrosion sodium aluminate solution that is α K=1.40 is for raw material, under the temperature of reaction of 70 DEG C, 1.5 parts of dispersion agents (AB8030 is sold in market) are added while adding the crystal seed of 1.25 parts of wet grindings, after stirring reaction 6h, the slurries of gained are carried out solid-liquid separation, washing, oven dry and impact grinding break up, impact grinding main frame frequency is 30HZ, grading machine frequency is 40HZ, finally obtain ultrafine powder aluminium hydroxide to pack, product cut size D
100for 7.8um, accompanying drawing 5 is shown in by product SEM photo.
Test example 1
Product by embodiment of the present invention 1-4 is applied under identical conditions in the cable formula on EVA basis, with ordinary hydrogen aluminum oxide for contrast, effect is done and illustrates, refer to table 1.
The representative formula of EVA cable is as follows:
The application performance data sheet of table 1 aluminum hydroxide product in EVA cable
Remarks: above Product processing is normal, material strip smooth surface, does not occur the problem foamed within the scope of the normal process temperature of EVA.
Can obviously be found out by above testing data, product of the present invention is after chemistry and physics two kinds of methods fundamentally solve the agglomeration traits of product from the microcosmic aspect of product, not only processing when adding the addition of 50% normally, being significantly improved in mechanical performance data, what is more important in the mobility of product be improved significantly, improve the working (machining) efficiency of modifying material product, to some extent solve the bridging problem of product blanking.
Claims (5)
1. the preparation method of a high-dispersion ultrafine aluminium hydroxide, it is characterized in that, with 100 parts of alumina contents be 220g/L ~ 260g/L, the solution Crater corrosion sodium aluminate solution that is α K=1.4 ~ 1.6 is for raw material, under the temperature of reaction of 55 ~ 75 DEG C, add 0.5 ~ 2 part of crystal seed, add 0.5 ~ 2.0 part of dispersed modifier simultaneously, after stirring reaction 6 ~ 11h, the slurries of gained are carried out solid-liquid separation, washing, oven dry and impact grinding break up, finally obtain ultrafine powder aluminium hydroxide, its D50=0.8 ~ 2um, D100 < 10um.
2. the preparation method of high-dispersion ultrafine aluminium hydroxide as claimed in claim 1, it is characterized in that, described crystal seed is wet milling process aluminium hydroxide seed, seed particle size D
100< 5 μm.
3. the preparation method of high-dispersion ultrafine aluminium hydroxide as claimed in claim 1, it is characterized in that, described dispersed modifier is Trisodium Citrate, silane A-151, amine hydroxybenzene, dispersion agent (AB8030) wherein one or more.
4. the preparation method of high-dispersion ultrafine aluminium hydroxide as claimed in claim 1, it is characterized in that, when impact grinding is broken up, impact grinding main frame frequency is 30 ~ 50HZ, and grading machine frequency is 25 ~ 45HZ.
5. the preparation method of the high-dispersion ultrafine aluminium hydroxide as described in as arbitrary in claim 1-4, it is characterized in that, , a kind of preparation method of high-dispersion ultrafine aluminium hydroxide, with 100 parts of alumina contents for 235g/L, solution Crater corrosion is the sodium aluminate solution of α K=1.52 is raw material, under the temperature of reaction of 65 DEG C, 1.2 parts of Trisodium Citrates are added while adding the crystal seed of 1.5 parts of wet grindings, after stirring reaction 8h, the slurries of gained are carried out solid-liquid separation, washing, oven dry and impact grinding are broken up, impact grinding main frame frequency is 40HZ, grading machine frequency is 35HZ, finally obtain ultrafine powder aluminium hydroxide to pack, product cut size D
100for 7um.
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Cited By (8)
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CN109082079A (en) * | 2018-07-03 | 2018-12-25 | 贵州大学 | A kind of method of relieving haperacidity coproduction electric stress control adhesive tape supporting material |
CN109437267A (en) * | 2018-12-03 | 2019-03-08 | 广西华银铝业有限公司 | A kind of decomposition method of Bayer process sodium aluminate solution |
CN110357134A (en) * | 2019-08-16 | 2019-10-22 | 山东省化工研究院 | A kind of aluminium hydroxide synthesis process size controlling method |
CN111099645A (en) * | 2019-12-23 | 2020-05-05 | 山东泰星新材料股份有限公司 | Preparation method of flower-shaped aluminum hydroxide for pouring sealant |
CN111807392A (en) * | 2020-06-28 | 2020-10-23 | 山东泰星新材料股份有限公司 | Preparation method of submicron-grade superfine aluminum hydroxide, product and application thereof |
CN114618646A (en) * | 2022-02-07 | 2022-06-14 | 中铝山东新材料有限公司 | Preparation method of superfine aluminum hydroxide micro powder |
CN114988448A (en) * | 2022-05-30 | 2022-09-02 | 洛阳职业技术学院 | Submicron aluminum hydroxide and preparation method thereof |
CN115818685A (en) * | 2021-09-15 | 2023-03-21 | 姜进涛 | Preparation method of spherical easily-dispersible alumina for diaphragm |
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2015
- 2015-11-20 CN CN201510817320.0A patent/CN105271336A/en active Pending
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109082079A (en) * | 2018-07-03 | 2018-12-25 | 贵州大学 | A kind of method of relieving haperacidity coproduction electric stress control adhesive tape supporting material |
CN109437267A (en) * | 2018-12-03 | 2019-03-08 | 广西华银铝业有限公司 | A kind of decomposition method of Bayer process sodium aluminate solution |
CN110357134A (en) * | 2019-08-16 | 2019-10-22 | 山东省化工研究院 | A kind of aluminium hydroxide synthesis process size controlling method |
CN110357134B (en) * | 2019-08-16 | 2021-08-06 | 山东省化工研究院 | Particle size control method in aluminum hydroxide synthesis process |
CN111099645A (en) * | 2019-12-23 | 2020-05-05 | 山东泰星新材料股份有限公司 | Preparation method of flower-shaped aluminum hydroxide for pouring sealant |
CN111099645B (en) * | 2019-12-23 | 2022-10-18 | 山东泰星新材料股份有限公司 | Preparation method of flower-shaped aluminum hydroxide for pouring sealant |
CN111807392A (en) * | 2020-06-28 | 2020-10-23 | 山东泰星新材料股份有限公司 | Preparation method of submicron-grade superfine aluminum hydroxide, product and application thereof |
CN115818685A (en) * | 2021-09-15 | 2023-03-21 | 姜进涛 | Preparation method of spherical easily-dispersible alumina for diaphragm |
CN114618646A (en) * | 2022-02-07 | 2022-06-14 | 中铝山东新材料有限公司 | Preparation method of superfine aluminum hydroxide micro powder |
CN114988448A (en) * | 2022-05-30 | 2022-09-02 | 洛阳职业技术学院 | Submicron aluminum hydroxide and preparation method thereof |
CN114988448B (en) * | 2022-05-30 | 2024-04-26 | 洛阳职业技术学院 | Submicron aluminum hydroxide and preparation method thereof |
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