CN105347367A - Preparing method of nanoscale magnesium hydroxide micropowder - Google Patents
Preparing method of nanoscale magnesium hydroxide micropowder Download PDFInfo
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- CN105347367A CN105347367A CN201510934128.XA CN201510934128A CN105347367A CN 105347367 A CN105347367 A CN 105347367A CN 201510934128 A CN201510934128 A CN 201510934128A CN 105347367 A CN105347367 A CN 105347367A
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- magnesium hydroxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
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- Crystallography & Structural Chemistry (AREA)
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparing method of nanoscale magnesium hydroxide micropowder. The preparing method comprises following steps in sequence: a) mixing a dispersant and a surfactant proportionally, dissolving in a liquid medium and forming dissolution liquid; b) reacting the dissolution liquid, magnesium oxide and a defoaming agent in a planetary ball mill in proportion to form nanoscale magnesium hydroxide suspension slurry; c) drying the suspension slurry by a spraying dryer, and sintering and dispersing to obtain the nanoscale magnesium hydroxide powder. The obtained nanoscale magnesium hydroxide micropowder is high in product yield and stable in quality, and the method has easily controlled reaction conditions and is suitable for industrialized production.
Description
Technical field
The present invention relates to the preparation method of magnesium hydroxide, particularly a kind of preparation method of nanometric magnesium hydroxide micro mist.
Background technology
Nanometric magnesium hydroxide is high because having purity, particle diameter is little, the excellent properties such as in-stiu coating modification can be carried out, can more uniformly be scattered in the rubber such as PA, PP, ABS, PVC, plastic prod, and significantly improve when affecting working strength hardly material fire-retardant, press down cigarette, the performance such as antidrip, be widely used in rubber-plastic elastomer, high-grade CABLE MATERIALS, in the high-end products such as household electrical appliance.
At present, conventional method has metal magnesium hydration method, brucite comminuting method, Chemical liquid deposition and bubble liquid-film method etc.Metal magnesium hydration method product purity is high, but cost is also high, and productive rate is low, and difficulty realizes suitability for industrialized production.The powder that brucite comminuting method obtains forms batch production, supply market, but because of the brucite mineral reserve resource-constrained of high-quality, consume energy high, the size of particle is generally 0.7-3 μm or larger, yardstick and distribution of shapes wide.According to Chemical liquid deposition principle, derive the multiple method such as direct precipitation method, precipitation-hydrothermal method, but all because of its product or purity is low or particle diameter is large or size distribution is wide and be more difficultly applied to industrial sector.
Comparative maturity, method that quality product is higher is air bubble liquid-membrane method, it has and suppresses to reunite, reduce water discharge, energy-saving and cost-reducing advantage, and product cut size and fractions distribution even, can guarantee often to criticize quality product identical.But air bubble liquid-membrane method is higher to processing parameter accuracy requirement, production process controls to acquire a certain degree of difficulty.
Summary of the invention
In order to overcome Problems existing in existing nanometric magnesium hydroxide technique, the invention provides a kind of preparation method of nanometric magnesium hydroxide micro mist.
The object of the invention is to be reached by following measures: the preparation method providing a kind of nanometric magnesium hydroxide micro mist, in turn includes the following steps: a) dispersion agent and tensio-active agent are mixed in proportion, is dissolved in liquid medium, form lysate; B) lysate, magnesium oxide and defoamer are reacted in proportion in planetary ball mill, form nanometric magnesium hydroxide suspension slurry; C) carry out drying to suspension slurry, sintering, breaks up, obtains nanometric magnesium hydroxide powder.
One preferred version is: dispersion agent used is the mixture of a kind of or arbitrary combination in polyoxyethylene glycol, citric acid or polyvinyl butyral acetal; Consumption and magnesium oxide weight ratio are (1 ~ 50): 1000.
One preferred version is: tensio-active agent used is one or both of Sodium dodecylbenzene sulfonate or sodium carboxymethylcellulose pyce; Consumption and magnesium oxide weight ratio are (1 ~ 50): 1000.
One preferred version is: defoamer used is one or both of octanol or glycerine; Consumption and magnesium oxide weight ratio are (1 ~ 50): 1000.
One preferred version is: balls grinding machine is planetary ball mill, and its rotating speed is between 150 ~ 400r/min, and Ball-milling Time is between 5 ~ 105 minutes, and ratio of grinding media to material is between 1.5 ~ 5.
One preferred version is: used medium is electronic grade ultrapure water, and temperature is between 75 ~ 99 DEG C.
One preferred version is: described drying adopts spray-drier, and its inlet temperature is between 200 ~ 280 DEG C, and air outlet temperature is between 95 ~ 115 DEG C, and spraying gun rotating speed is between 8000 ~ 14000 turns.
One preferred version is: described sintering temperature is 200 ~ 320 DEG C, stops 1 ~ 10 hour, and during intensification, per minute heats up 3 ~ 10 degrees Celsius.
One preferred version for: described in break up the equipment of use for airflow milling.
Beneficial effect: product production of the present invention is high, steady quality, and easy control of reaction conditions, be applicable to suitability for industrialized production.
Embodiment
Below by embodiment, the present invention is described in detail.
The invention provides a kind of preparation method of nanometric magnesium hydroxide micro mist, in turn include the following steps: a) dispersion agent and tensio-active agent are mixed in proportion, be dissolved in liquid medium, form lysate; B) lysate, magnesium oxide and defoamer are reacted in proportion in planetary ball mill, form nanometric magnesium hydroxide suspension slurry; C) carry out drying to suspension slurry, sintering, breaks up, obtains nanometric magnesium hydroxide powder.
One preferred version is: dispersion agent used is the mixture of a kind of or arbitrary combination in polyoxyethylene glycol, citric acid or polyvinyl butyral acetal; Consumption and magnesium oxide weight ratio are (1 ~ 50): 1000.
One preferred version is: tensio-active agent used is one or both of Sodium dodecylbenzene sulfonate or sodium carboxymethylcellulose pyce; Consumption and magnesium oxide weight ratio are (1 ~ 50): 1000.
One preferred version is: defoamer used is one or both of octanol or glycerine; Consumption and magnesium oxide weight ratio are (1 ~ 50): 1000.
One preferred version is: balls grinding machine is planetary ball mill, and its rotating speed is between 150 ~ 400r/min, and Ball-milling Time is between 5 ~ 105 minutes, and ratio of grinding media to material is between 1.5 ~ 5.
One preferred version is: used medium is electronic grade ultrapure water, and temperature is between 75 ~ 99 DEG C.
One preferred version is: described drying adopts spray-drier, and its inlet temperature is between 200 ~ 280 DEG C, and air outlet temperature is between 95 ~ 115 DEG C, and spraying gun rotating speed is between 8000 ~ 14000 turns.
One preferred version is: described sintering temperature is 200 ~ 320 DEG C, stops 1 ~ 10 hour, and during intensification, per minute heats up 3 ~ 10 degrees Celsius.
One preferred version for: described in break up the equipment of use for airflow milling.
Embodiment
A) by 0.5g polyvinyl butyral acetal, 0.3g Sodium dodecylbenzene sulfonate in 500ml pure water, dissolve after keep temperature be 90 DEG C, prepare out lysate;
B) successively 100g high-purity magnesium oxide, lysate, 2ml glycerine are added ball grinder.Ball radius is 5mm, 200g, and drum's speed of rotation is 350r/min, and ball milling 30 minutes, can obtain nano-sized magnesium hydroxide suspended nitride;
C) utilize spray-drier to carry out drying to slurry, obtain loose spheroidal particle, particle diameter is between 30 ~ 60 μm.Spray-drier inlet temperature is 230 DEG C, and air outlet temperature is 105 DEG C, and per minute heats up 5 DEG C, finally stops at 320 DEG C and sinters for 3 hours, make the organic chemical reagent mixed be decomposed into H
2o and CO
2, volatilize away from powder;
D) loose particle is broken up through airflow milling, Magnesium Hydroxide Nano-particles.
Above content is the further description done the present invention in conjunction with optimal technical scheme, can not assert that the concrete enforcement of invention is only limitted to these explanations.Concerning general technical staff of the technical field of the invention, under the prerequisite not departing from design of the present invention, simple deduction and replacement can also be made, all should be considered as protection scope of the present invention.
Claims (9)
1. a preparation method for nanometric magnesium hydroxide micro mist, is characterized in that, in turn includes the following steps: a) dispersion agent and tensio-active agent are mixed in proportion, is dissolved in liquid medium, forms lysate; B) lysate, magnesium oxide and defoamer are reacted in proportion in planetary ball mill, form nanometric magnesium hydroxide suspension slurry; C) carry out drying to suspension slurry, sintering, breaks up, obtains nanometric magnesium hydroxide powder.
2. the preparation method of a kind of nanometric magnesium hydroxide micro mist according to claim 1, is characterized in that, dispersion agent used is the mixture of a kind of or arbitrary combination in polyoxyethylene glycol, citric acid or polyvinyl butyral acetal; Consumption and magnesium oxide weight ratio are (1 ~ 50): 1000.
3. the preparation method of a kind of nanometric magnesium hydroxide micro mist according to claim 1, is characterized in that, tensio-active agent used is one or both of Sodium dodecylbenzene sulfonate or sodium carboxymethylcellulose pyce; Consumption and magnesium oxide weight ratio are (1 ~ 50): 1000.
4. the preparation method of a kind of nanometric magnesium hydroxide micro mist according to claim 1, is characterized in that, defoamer used is one or both of octanol or glycerine; Consumption and magnesium oxide weight ratio are (1 ~ 50): 1000.
5. the preparation method of a kind of nanometric magnesium hydroxide micro mist according to claim 1, it is characterized in that, balls grinding machine is planetary ball mill, and its rotating speed is between 150 ~ 400r/min, Ball-milling Time is between 5 ~ 105 minutes, and ratio of grinding media to material is between 1.5 ~ 5.
6. the preparation method of a kind of nanometric magnesium hydroxide micro mist according to claim 1, is characterized in that, used medium is electronic grade ultrapure water, and temperature is between 75 ~ 99 DEG C.
7. the preparation method of a kind of nanometric magnesium hydroxide micro mist according to claim 1, it is characterized in that, described drying adopts spray-drier, and its inlet temperature is between 200 ~ 280 DEG C, air outlet temperature is between 95 ~ 115 DEG C, and spraying gun rotating speed is between 8000 ~ 14000 turns.
8. the preparation method of a kind of nanometric magnesium hydroxide micro mist according to claim 1, is characterized in that, described sintering temperature is 200 ~ 320 DEG C, stops 1 ~ 10 hour, and during intensification, per minute heats up 3 ~ 10 degrees Celsius.
9. the preparation method of a kind of nanometric magnesium hydroxide micro mist according to claim 1, is characterized in that, described in break up the equipment of use for airflow milling.
Priority Applications (1)
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| CN201510934128.XA CN105347367A (en) | 2015-12-15 | 2015-12-15 | Preparing method of nanoscale magnesium hydroxide micropowder |
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| CN201510934128.XA CN105347367A (en) | 2015-12-15 | 2015-12-15 | Preparing method of nanoscale magnesium hydroxide micropowder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115748A (en) * | 2016-06-16 | 2016-11-16 | 东升新材料（山东）有限公司 | A kind of method of preparing super fine magnesium hydroxide by wet method slurry |
| CN107117586A (en) * | 2017-04-25 | 2017-09-01 | 江苏师范大学 | It is a kind of to improve the method that chemical precipitation method prepares oxide powder dispersiveness |
| CN108706612A (en) * | 2018-07-04 | 2018-10-26 | 河南师范大学 | A kind of method that mechanical ball mill prepares nano-sized magnesium hydroxide |
| CN114213875A (en) * | 2021-12-24 | 2022-03-22 | 大连理工大学 | High-stability magnesium hydroxide suspension and preparation method thereof |
-
2015
- 2015-12-15 CN CN201510934128.XA patent/CN105347367A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115748A (en) * | 2016-06-16 | 2016-11-16 | 东升新材料（山东）有限公司 | A kind of method of preparing super fine magnesium hydroxide by wet method slurry |
| CN106115748B (en) * | 2016-06-16 | 2018-01-09 | 东升新材料（山东）有限公司 | A kind of method of preparing super fine magnesium hydroxide by wet method slurry |
| CN107117586A (en) * | 2017-04-25 | 2017-09-01 | 江苏师范大学 | It is a kind of to improve the method that chemical precipitation method prepares oxide powder dispersiveness |
| CN107117586B (en) * | 2017-04-25 | 2019-05-31 | 新沂市中大石英科技有限公司 | A method of it improving chemical precipitation method and prepares oxide powder dispersibility |
| CN108706612A (en) * | 2018-07-04 | 2018-10-26 | 河南师范大学 | A kind of method that mechanical ball mill prepares nano-sized magnesium hydroxide |
| CN114213875A (en) * | 2021-12-24 | 2022-03-22 | 大连理工大学 | High-stability magnesium hydroxide suspension and preparation method thereof |
| CN114213875B (en) * | 2021-12-24 | 2022-05-20 | 大连理工大学 | High-stability magnesium hydroxide suspension and preparation method thereof |
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