CN103849924B - A kind of method utilizing alkali magnesium sulfate crystal whisker to prepare nano-sized magnesium hydroxide whisker - Google Patents

A kind of method utilizing alkali magnesium sulfate crystal whisker to prepare nano-sized magnesium hydroxide whisker Download PDF

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CN103849924B
CN103849924B CN201410048281.8A CN201410048281A CN103849924B CN 103849924 B CN103849924 B CN 103849924B CN 201410048281 A CN201410048281 A CN 201410048281A CN 103849924 B CN103849924 B CN 103849924B
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whisker
magnesium sulfate
sulfate crystal
alkali magnesium
type alkali
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CN103849924A (en
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姜玉芝
张忠阳
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Nantong Shuangyao Stamping Co ltd
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Shenyang Ligong University
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Abstract

A kind of method utilizing alkali magnesium sulfate crystal whisker to prepare nano-sized magnesium hydroxide whisker, it is with 153 type alkali magnesium sulfate crystal whiskers for raw material, in 153 type alkali magnesium sulfate crystal whiskers, add distilled water be configured to the initial slip of 153 type alkali magnesium sulfate crystal whiskers, add sodium hydroxide that concentration is 1.0-4.0mol/L and auxiliary agent sodium stearate makes base material;The sodium hydroxide solution addition of 1.0-4.0mol/L is pressed the charge ratio of Na0H:153 type alkali magnesium sulfate crystal whisker=2-4.5:1 and is added;Sodium stearate addition is the 1-5% of 135 type alkali magnesium sulfate crystal whisker quality;Being put into by base material in autoclave, when reactor temperature reaches 160-200 DEG C, be incubated 1-5h, then turn off heating and stirring, air cooling, to room temperature, through conventional disperse, washing, filtration and dry, to obtain final product.Present invention process is simple, reduced investment, easy industrialization, it is thus achieved that high financial profit.

Description

A kind of method utilizing alkali magnesium sulfate crystal whisker to prepare nano-sized magnesium hydroxide whisker
Technical field
This invention belongs to inorganic non-metallic technical field of powdered material preparation, is specially a kind of method utilizing alkali magnesium sulfate crystal whisker to prepare nano-sized magnesium hydroxide whisker.
Background technology
The research and development of multifunctional material and using particularly are paid close attention to by 21 century people, and material is multi-functional and environmental-protecting performance requires more and more higher, therefore quality better, the many environmental protections of function high end materials be one of the research and development of current material circle and Main way of producing.And nano-sized magnesium hydroxide whisker has higher added value because of it, it has also become one of study hotspot of fire retardant and Material Field.
Ordinary hydrogen magnesium oxide product adds to as fire retardant mainly two shortcomings in polymer: the addition of magnesium hydroxide when being play flame retardant effect needs to play very greatly good flame retardant effect;Two is poor with the compatibility of polymeric matrix, and the composite materials property of preparation is poor, it is impossible to meet the Material Field requirement to its mechanical property.Generally to obtain good flame retardant effect, the addition of magnesium hydroxide generally requires and reaches more than 50 parts (whisker quality/100 substrate qualities), this will be substantially reduced mechanical property and the processing characteristics of composite, be extremely difficult to actually used prescription.So being one of the key issue of solution of being eager at present improving the mechanical property not changing or significantly reducing matrix material itself while magnesium hydroxide flame retardant effect.Research shows, magnesium hydroxide is notable to the Effect on Mechanical Properties of composite with the adhesive ability of polymeric matrix and the reunion degree of magnesium hydroxide, and magnesium hydroxide crystal pattern is one of key factor of these influence factors.Magnesium hydroxide relative to other sizes, nano-sized magnesium hydroxide has better dispersibility in material matrix, the mechanical property of matrix material is had good reinforcing effect by the special magnesium hydroxide crystal of pattern, and the hot strength of threadiness magnesium hydroxide/polymer composites and impact strength are obviously higher than spherical magnesium hydroxide/polymer composites.Because nano-sized magnesium hydroxide whisker has the performances such as good heat-resisting, heat insulation, adiabatic, enhancing, along with constantly researching and developing and perfect of nano-sized magnesium hydroxide whisker, its application prospect will be more extensive, so the research of the preparation and dispersibility carrying out nano-sized magnesium hydroxide whisker has very great and realistic meaning.
Summary of the invention
The purpose of the present invention, is to provide a kind of method utilizing alkali magnesium sulfate crystal whisker to prepare nano-sized magnesium hydroxide whisker.
This invention is with 153 type alkali magnesium sulfate crystal whisker (MgSO4·5Mg(OH)2·3H2O) (alkali magnesium sulfate crystal whisker is called for short MOSW) is raw material, with sodium hydroxide for precipitant, adopts hydro-thermal method to prepare nano-sized magnesium hydroxide whisker.Through test of many times, finally invented fairly simple nano-sized magnesium hydroxide crystal whisker preparation method, with the product purity that a process for preparing Whisker Content high, single be whisker sum 80%, whisker average diameter 85nm, draw ratio > 100, whisker morphology uniform.
The technical scheme is that for achieving the above object
A kind of method utilizing alkali magnesium sulfate crystal whisker to prepare nano-sized magnesium hydroxide whisker, comprises the steps:
(1) with 153 type alkali magnesium sulfate crystal whiskers for raw material, adding distilled water and be configured to the initial slip of 153 type alkali magnesium sulfate crystal whiskers, initial pulp density is 0.01-0.05mol/kg.
(2) initial slurry prepared to step (1) adds sodium hydroxide and the auxiliary agent sodium stearate that concentration is 1.0-4.0mol/L, make base material, wherein the sodium hydroxide solution addition of 1.0-4.0mol/L is add by the charge ratio of Na0H:153 type alkali magnesium sulfate crystal whisker=2-4.5:1 with molar ratio computing, and sodium stearate addition is the 1-5% of 153 type alkali magnesium sulfate crystal whisker quality.
(3) base material that step (2) is configured to is put in autoclave, intensification limit, limit is stirred with 100-500r/min speed, when reactor temperature reaches 160-200 DEG C, constant temperature and pressure insulation 1-5h, then turning off heating and stirring, air cooling, to room temperature, takes out synthetic product in autoreaction still, through conventional disperse, washing, filtration and dry, namely obtain nano-sized magnesium hydroxide whisker.
The pattern of above-mentioned nano-sized magnesium hydroxide whisker is draw ratio > 100, average diameter is 85nm, and single Whisker Content reaches 80%.
Further illustrating technique scheme:
One, prepare in nano-sized magnesium hydroxide whisker process in enforcement this invention creation, the major parameter affecting product quality includes the pattern of 153 type alkali magnesium sulfate crystal whiskers, the initial pulp density of alkali magnesium sulfate crystal whisker, NaOH:MOSW mol ratio, reaction temperature, response time, the factor such as mixing speed, additive types and addition.
(1) 153 type alkali magnesium sulfate crystal whisker pattern.The formation of nano-sized magnesium hydroxide whisker is had critical impact by the pattern of 153 type alkali magnesium sulfate crystal whisker raw materials, wherein choose diameter of whiskers≤500nm, draw ratio > 100, smooth surface, the 153 type alkali magnesium sulfate crystal whiskers that straight, very thin, pattern is uniform, dispersion effect is good, the nano-sized magnesium hydroxide whisker prepared is more satisfactory.
(2) the 153 initial pulp densities of type alkali magnesium sulfate crystal whisker.The major diameter of 153 type alkali magnesium sulfate crystal whiskers is relatively larger, and dispersibility is better, containing 3 water of crystallization in molecule, when preparing into the initial slip of alkali magnesium sulfate together with distilled water, whisker is dispersed in water, after its molality reaches certain value, and agitated pasty state slip.The pattern of product can be affected if the molality of this kind of slip is on the low side, too high will affect products collection efficiency.In order to make sodium hydrate aqueous solution mix homogeneously with alkali magnesium sulfate slip, reacting fully and carry out, the initial pulp density of the alkali magnesium sulfate crystal whisker that the present invention adopts is 0.01-0.05mol/kg.
(3) NaOH:MOSW mol ratio.In order to make the pattern more expansion of the nano-sized magnesium hydroxide whisker of synthesis, yield is higher, should NaOH:MOSW mol ratio be controlled within the specific limits, and the two mol ratio is too low can not form whisker, and the diameter of whiskers formed time too high is thick, and agglomeration is obvious.In order to make whisker reach the pattern of the best, the NaOH:MOSW mol ratio that the present invention adopts is 2.0-4.5:1.
(4) auxiliary agent kind and addition.The preparation to nano-sized magnesium hydroxide whisker that adds of auxiliary agent plays the effect of key, when adopting sodium stearate as dispersing aid, in the process of preparation, sodium stearate addition is sodium stearate: MOSW mass ratio is 1-3%, synthesized magnesium hydroxide crystal whisker diameter is nanoscale, pattern expansion, diameter of whiskers is uniform.
(5) reaction temperature.In nano-sized magnesium hydroxide preparation process, reaction temperature should be strict controlled in certain limit, the too low formation being unfavorable for whisker of temperature, temperature is too high affect whisker dispersibility while also result in the waste of the energy.The nano-sized magnesium hydroxide whisker morphology obtained when 160-200 DEG C in the present invention is more satisfactory, and major diameter is relatively larger, and the thinner average diameter of diameter of whiskers is 85nm, and the expansion of whisker is better, and tiny Whisker Content is relatively low.
(6) response time.Synthesis product morphology and phase structure are all had direct impact by the hydro-thermal reaction time.The hydro-thermal reaction time can not be too short, and being formed of whisker needs the sufficient response time, but the expansion of response time long whisker product morphology can decrease, and diameter of whiskers is thicker.At 160-200 DEG C, reaching 1-5h between when reacted, whisker morphology is more satisfactory, and major diameter is relatively larger, whisker expansion.X-ray diffractometer is utilized to carry out phase structure analysis for synthetic product, result shows, the X-ray diffraction peak d value of its synthetic product and the d value one_to_one corresponding of PDF74-2220 magnesium hydroxide standard card, and peak shape is sharp-pointed, free from admixture peak exists, and illustrates that product is all the magnesium hydroxide of complete crystallization.
(7) mixing speed.In order to enable hydro-thermal reaction to carry out uniformly, being stirred all the time for proceeding to alkali magnesium sulfate crystal whisker in reactor and sodium hydroxide mixed solution in course of reaction, mixing speed should control within the specific limits.When mixing speed is 100-500r/min, it is possible to prepare the nano-sized magnesium hydroxide whisker of more satisfactory pattern.
Adopt S-3400N sem observation Hydrothermal Synthesis product morphology, SEM map analysis measure diameter and the length of fibrous product, calculate the draw ratio of product;Utilize the thing phase composition of UltimaIV type x-ray diffractometer detection synthetic product.
Two, the preparation method of 153 type alkali magnesium sulfate crystal whisker raw materials:
153 type alkali magnesium sulfate crystal whisker raw material preparation flows are: accurately weigh certain mass extra light calcined magnesia powder mull to 74 μm, add deionized water, it is sufficiently stirred for and is configured to the magnesium oxide primary response slip that concentration is 0.01-0.05mol/kg, the sulfuric acid solution of 1mol/L concentration is joined in slip, proceed to after fully dispersed in autoclave, it is warmed up to 170-200 DEG C, insulation 2.0-6.0h, close heating power supply and stop stirring, product is cooled to room temperature with still sky, sampling, dispersion, washing, filter, dry, namely 153 type alkali magnesium sulfate crystal whisker (MgSO are obtained4·5Mg(OH)2·3H2O), its diameter of whiskers≤500nm, draw ratio > 100, smooth surface, straight, very thin.
Compared with the existing technical method preparing nano-sized magnesium hydroxide whisker, this invention has the advantage that
(1) raw material sources are extensive.China is one of country that high-quality magnesite reserves are maximum.With it for raw material, can obviously reduce the preparation cost of nano-sized magnesium hydroxide whisker.
(2) technique is simple.Whole technical process is divided into two big operations, and each operation needs the relevant parameter controlled fewer, simple to operate.
(3) equipment is produced more single.Roaster, autoclave and drying equipment are the three main bodies equipment in whole preparation technology, and all the other are that the large-scale hopper of acid and alkali-resistance, mixing and mixing plant etc., therefore small investment, it is easy to industrialization, and main equipment easily realize automatically controlling.
(4) the nano-sized magnesium hydroxide whisker that this method produces is utilized to fill the domestic gaps, dose the consumption that both can reduce rubber, plastics in the high molecular polymer such as rubber, plastics, reduce goods cost, it is remarkably improved again the fire-retardant of material and mechanical mechanics property, reduce the generation of fire incident, reduce unnecessary loss for society, improve people's security and quality of life, it is achieved environment-friendly flame retardant.
Detailed description of the invention
Embodiment 1
Utilizing the magnesite that is produced from somewhere, Liaoning is raw material, prepares nano-sized magnesium hydroxide whisker.
Accurately weigh the oxide of high activity magnesium dust (being ground to 74 μm) after the calcining of 2.4g magnesite, add 1985mL deionized water, after stirring, adding 15mL concentration is the sulfuric acid solution of 1.0mol/L, making concentration is the 0.03mol/kg initial slip of initial oxidation magnesium, proceed to after mix homogeneously in autoclave, when being warmed up to 180 DEG C, insulation 4h, stop heating and stirring is cooled to room temperature with reactor sky, sampling, disperse, filter, dry, namely obtain 153 type alkali magnesium sulfate crystal whiskers, molecular formula is MgSO4·5Mg(OH)2·3H2O.This alkali magnesium sulfate crystal whisker stock diameter≤500nm, draw ratio > 100, smooth surface, straight, very thin, reach 98.17% through quantitative chemical analysis purity.
The alkali magnesium sulfate crystal whisker prepared is added distilled water and is configured to the initial slip that molality is 0.02mol/kg, then sodium hydrate aqueous solution is joined in alkali magnesium sulfate crystal whisker slip according to the addition that NaOH:MOSW mol ratio is 3:1, press sodium stearate: the amount of MOSW mass ratio 2% adds sodium stearate simultaneously, proceed to afterwards by evenly mixing in autoclave, with mixing speed for 100r/min warming while stirring, when temperature in the kettle is raised to 180 DEG C, constant temperature and pressure insulation 1h, then turn off heating and stirring, naturally cool to room temperature.Autoreaction still is interior takes out reaction product, through dispersion, washing, filtration, dries, namely obtains nano-sized magnesium hydroxide whisker.
The pattern of the obtained synthetic product of present study and thing phase composition, adopt XRD spectra and SEM scanning electron microscope test to analyze, it is shown that synthetic product pattern is in threadiness, length is relatively big, and whisker average diameter 84nm belongs to nanoscale;Draw ratio > 100, and very thin uniformly.Main X-diffraction maximum d value (descending) of synthetic product is respectively as follows: 4.7680,2.7254,2.3661,1.7944,1.4942 and 1.3729, d value one_to_one corresponding with PDF74-2220 magnesium hydroxide standard card, peak shape is sharp-pointed, and free from admixture peak exists.Measurement results shows that Hydrothermal Synthesis product is nano-sized magnesium hydroxide whisker, and complete crystallization, purity reaches more than 98.0%.

Claims (2)

1. one kind utilizes the method that alkali magnesium sulfate crystal whisker prepares nano-sized magnesium hydroxide whisker, it is characterised in that: comprise the steps:
(1) with 153 type alkali magnesium sulfate crystal whiskers for raw material, wherein 153 type alkali magnesium sulfate crystal whisker diameters≤500nm, draw ratio 100, smooth surface, straight, very thin, adding distilled water in 153 type alkali magnesium sulfate crystal whiskers and be configured to the initial slip of 153 type alkali magnesium sulfate crystal whiskers, initial pulp density is 0.01-0.05mol/kg;
(2) initial slurry prepared to step (1) adds sodium hydroxide that concentration is 1.0-4.0mol/L and auxiliary agent sodium stearate makes base material;The sodium hydroxide solution addition of 1.0-4.0mol/L is pressed, with molar ratio computing, the charge ratio that NaOH:153 type alkali magnesium sulfate crystal whisker is 2-4.5:1 and is added;Sodium stearate addition is the 1-5% of 153 type alkali magnesium sulfate crystal whisker quality;
(3) base material that step (2) is configured to is put in autoclave, intensification limit, limit is stirred with 100-500r/min speed, when reactor temperature reaches 160-200 DEG C, constant temperature and pressure insulation 1-5h, then turn off heating and stirring, naturally cool to room temperature, autoreaction still takes out synthetic product, through conventional disperse, washing, filtration and dry, obtain nano-sized magnesium hydroxide whisker.
2. a kind of method utilizing alkali magnesium sulfate crystal whisker to prepare nano-sized magnesium hydroxide whisker according to claim 1, it is characterised in that: the pattern of above-mentioned nano-sized magnesium hydroxide whisker is draw ratio 100, average diameter is 85nm, and single Whisker Content reaches 80%.
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CN104593867A (en) * 2014-12-25 2015-05-06 武汉工程大学 Method for preparing in-situ modified nano-magnesium hydroxide whiskers by taking phosphate tailings as raw materials
CN105256405B (en) * 2015-09-17 2017-07-28 南京工业大学 The method that magnesia aquation method prepares fibrous magnesium hydroxide
CN107673380B (en) * 2017-09-29 2019-05-10 中国科学院青海盐湖研究所 Alkali magnesium sulfate nano wire and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
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
CN1458066A (en) * 2002-05-17 2003-11-26 隗学礼 Process for preparing magnesium hydroxide whisker
CN1884633A (en) * 2006-05-31 2006-12-27 东北大学 Method for magnesium hydroxide whisker using giobertite as material
CN102877115A (en) * 2012-10-10 2013-01-16 中国科学院福建物质结构研究所 Preparation method of whisker-shaped magnesium hydroxide

Patent Citations (4)

* Cited by examiner, † Cited by third party
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
CN1458066A (en) * 2002-05-17 2003-11-26 隗学礼 Process for preparing magnesium hydroxide whisker
CN1884633A (en) * 2006-05-31 2006-12-27 东北大学 Method for magnesium hydroxide whisker using giobertite as material
CN102877115A (en) * 2012-10-10 2013-01-16 中国科学院福建物质结构研究所 Preparation method of whisker-shaped magnesium hydroxide

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
"功能化氢氧化镁晶须的制备与性能";李征征;《中国硕士学位论文全文数据库 工程科技I辑》;20090915(第9期);第23页第2段,第32页第2.4部分 *
"氢氧化镁晶须制备研究";姜玉芝等;《矿冶》;20060630;第15卷(第2期);第44-47页 *
"氢氧化镁纳米棒的制备和干燥动力学研究";云丽娜;《中国硕士学位论文全文数据库 工程科技I辑》;20080815(第8期);第44页第3.1.7部分 *

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