CN103159236A - Production method of environmental-protective grade magnesium hydroxide - Google Patents
Production method of environmental-protective grade magnesium hydroxide Download PDFInfo
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- CN103159236A CN103159236A CN2011104046937A CN201110404693A CN103159236A CN 103159236 A CN103159236 A CN 103159236A CN 2011104046937 A CN2011104046937 A CN 2011104046937A CN 201110404693 A CN201110404693 A CN 201110404693A CN 103159236 A CN103159236 A CN 103159236A
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Abstract
A production method of environmental-protective grade magnesium hydroxide is characterized in that the method comprises mixing industrial magnesium oxide and water with a mass ratio of 1 : 20 to 1 : 70, dispersing by ultrasonic for 30 minutes under a frequency of 50 Hz, adding a catalyst with an amount of 0.5-5 % by mass of water and a dispersant with an amount of 0.05-0.5 % by mass of the water, stirring the solution in a constant-temperature water bath, reacting for 2-12 hours under a temperature of 40-90 DEG C, after the reaction, standing, filtering with a pump and drying to a constant weight, immersing the product in anhydrous alcohol, re-drying to a constant weight, putting the product into a muffle furnace, roasting for 2.5 hours under 750 DEG C, taking out and cooling to obtain the finish product. The invention aims at providing a production method of high-quality and environmental-protective grade magnesium hydroxide with low cost and low energy consumption, so that the technology can be widely used.
Description
Technical field
The present invention relates to field of inorganic chemical engineering, be specifically related to a kind of technology of technical grade magnesium oxide aquation production environmental protection level magnesium hydroxide.
Background technology
Along with the development of China's industry, the environment of the mankind being depended on for existence by waste liquid and the waste gas of the discharging of the industries such as metallurgy, chemical industry, pharmacy has caused serious threat, how effectively to process this pollutant matter, becomes one of present problem demanding prompt solution.Based on the needs of present environment protection and the new millennium people new demand for the environmental treatment agent; be applied to some strong alkaline substances in field of Environment Protection such as the usage quantity of caustic soda, soda ash and lime and gradually reduce, and then the magnesium hydroxide that is more met environmental requirement and have strong absorption and shock-absorbing capacity replaces.Environmental protection level magnesium hydroxide is the green safety environmental treatment agent that is called as " the third alkali ", have the characteristics such as the use of processing is safe, nontoxic, non-corrosiveness, heavy metal wastewater thereby, dyeing waste water, acid waste water, flue gas desulfurization etc. are all had good treatment effect.
At present domestic production research to magnesium hydroxide mainly concentrates in the production application of fire retardant, and it is ripe that its technical development is tending towards, and less to production, the applied research of environmental protection level magnesium hydroxide.Traditional magnesium hydroxide preparation method has magnesium salts and the alkali reaction method of growing up, and natural mineral is pulverized method and magnesium oxide aquation method.Wherein comminuting method efficient is lower, energy consumption is large, and the products obtained therefrom particle is thicker, broad particle distribution, and the high and resource of foreign matter content is restricted, and the standby magnesium hydroxide of the legal system of growing up reaches balance at cost and difficult quality.Magnesium oxide aquation method is a kind of ancient technique, and its source is most to be obtained by calcinings such as magnesite, rhombspars, and China is magnesium resource big country, have abundant magnesium ore resources, so raw material sources is extensive, and cost is lower.The technique of the method is simple simultaneously, the production process environmentally safe, and the magnesium hydroxide specific surface area of using the magnesium oxide preparation is large, and absorption property is good, can be widely used in field of Environment Protection.
But still there is some problems in the standby magnesium hydroxide of traditional magnesium oxide aquation legal system, and its manufacturing condition is higher, energy consumption is large, therefore, can apply on a large scale in order to make this method, also needs the method is carried out certain technological improvement.
Summary of the invention
The object of the present invention is to provide a kind of low cost, less energy-consumption, the production technology of high quality environmental protection level magnesium hydroxide, thus this technology is used widely.
For achieving the above object, the present invention adopts technical scheme:
a kind of environmental protection level magnesium hydroxide production method, it is characterized in that: the industrial magnesium oxide that it is 1:20～1:70 that described method comprises mass ratio mixes with water, ultra-sonic dispersion 30min under the 50Hz frequency, then add the catalyzer that accounts for quality 0.5%～5% and the dispersion agent that accounts for quality 0.05%～0.5%, solution is placed in water bath with thermostatic control to be stirred, react 2h～12h at the temperature of 40 ℃～90 ℃, reaction finishes by standing, suction filtration, be dried to constant weight, product is immersed in dehydrated alcohol, again be dried to constant weight, then product is placed in retort furnace, 750 ℃ of calcining 2.5h, cooling getting final product after taking out.
Described catalyzer is at least a in ammonium formiate, magnesium acetate, triethylenediamine, vulkacit H.
Described dispersion agent is that a class is the polyalcohols material.
A described class is that the polyalcohols material is sucrose ester, polyoxyethylene glycol, spans or Tweens.
Described industrial magnesium oxide is light magnesium oxide, has better activity, can be obtained by the magnesite calcining.
The magnesium hydroxide purity of preparation is high, granularity is little, specific surface area is large, the adsorption-flocculation ability is good, and all kinds of water pollutant matter are had good treatment effect.
Products obtained therefrom is applied to the reactive black treatment of dyeing wastewater, and percent of decolourization is all more than 95%.
Environmental protection level magnesium hydroxide production technology of the present invention, equipment is simple, and is easy to operate, and raw material sources are extensive, greatly reduce production cost under the prerequisite that guarantees the aquation rate, quality product reaches III class environmental protection level magnesium hydroxide technical indicator in national HG/T3607-2007 proposed standard.This method has solved the high problem of magnesium oxide aquation processing condition simultaneously, for large-scale explained hereafter provides possibility.
Description of drawings:
Fig. 1 is magnesium hydroxide SEM figure after the magnesium oxide aquation under best hydrating condition;
Fig. 2 is product magnesium hydroxide XRD figure under best hydrating condition;
Fig. 3 is that the decolorizing printing and dyeing waste water rate is with magnesium hydroxide dosage variation relation figure.
Embodiment:
Under cold condition, magnesian aquation rate is very low, and the product granularity of preparation is larger.The contriver finds, if add a certain amount of catalyzer and dispersion agent in reaction process, can accelerating oxidation magnesium and the speed of reaction of water, and improve magnesian aquation rate, reduce simultaneously the product particle diameter.
The present invention adopts orthogonal experiment design to determine optimum reaction condition, and with the product that makes to the dyeing waste water processing of decolouring.
Experimental technique of the present invention is as follows:
(1) after being mixed with the ratio of mass ratio 1:20～1:70 with water, pours in there-necked flask in magnesium oxide, ultra-sonic dispersion 30min under the 50Hz frequency, add subsequently the catalyzer that accounts for quality 0.5-5% and the dispersion agent that accounts for quality 0.05%～0.5%, be placed in water bath with thermostatic control and stir, react 2h～12h at the temperature of 40 ℃～90 ℃.
Catalyzer is for being ammonium formiate, magnesium acetate, triethylenediamine, at least a in vulkacit H; Dispersion agent is selected a polynary polyalcohols material of class, sucrose ester, polyoxyethylene glycol, spans or Tweens.
(2) reaction is standing with the hydrated product that obtains after finishing, and suction filtration is with being placed on oven drying to constant weight; Be placed in again retort furnace and calcine, cooling after taking out, weigh.Calculate the aquation rate of product.
(3) get the magnesium hydroxide of producing under optimal conditions and be added in a certain amount of dyeing waste water, after magnetic agitation, standing sedimentation, get supernatant liquor and measure its colourity, calculate its percent of decolourization.
Test described aquation rate calculation formula as follows:
Aquation rate ﹪=
* 100 ﹪,
Wherein:
Weight before the dry fully rear calcining of-hydrated product;
Test described percent of decolourization calculation formula as follows:
---the colourity (doubly) after decolouring;
Aquation gained magnesium hydroxide stereoscan photograph under the optimum reaction condition as Fig. 1, can find out that the magnesium hydroxide pattern is rendered as sheet structure, and powder granule is less.This is to have improved the degree of supersaturation of solution owing to adding catalyzer in solution, thereby has accelerated the nucleation rate of magnesium hydroxide, makes the magnesium hydroxide particle of generation tiny, and specific surface area increases; Add simultaneously dispersion agent in solution effectively to be adsorbed on magnesium hydroxide crystallite surface, reduce product the surface can, and by Coulomb repulsion effect and space steric effect, avoid particle to grow up and reunion, thereby prepared sizes are little, the magnesium hydrate powder of good dispersity.
X-ray diffractogram from magnesium hydroxide product, as Fig. 2, can find out, hydrated product produces strong diffraction peak at 18.6 °, 37.9 °, 50.7 °, 58.6 °, 62 °, consistent with the diffraction peak in magnesium hydroxide standard spectrogram (PDF82-2353), only at an impurity peaks of 44 ° of appearance, this peak is caused by unhydrated magnesium oxide, so the purity of magnesium hydroxide is higher.
Processing for dyeing waste water, as can be seen from Figure 3, along with the increase of magnesium hydroxide dosage, magnesium hydroxide sharply rises to the decolorizing effect of dyeing waste water, after the concentration of magnesium hydroxide reached certain value, magnesium hydroxide solution no longer changed the useless decolorizing effect of printing and dyeing.
The present invention is described in detail below in conjunction with specific embodiment:
Embodiment 1:
With light magnesium oxide and water in mass ratio the 1:20 ratio mix, pour in there-necked flask ultra-sonic dispersion 30min under the 50Hz frequency into; Add subsequently the ammonium formiate that accounts for quality 0.5% and account for quality 0.05% sucrose ester, being placed in 40 ℃ of waters bath with thermostatic control and stirring, reaction 2h;
After reaction finishes, ultra-sonic dispersion after hydrated product is taken out, thin up, standing, suction filtration is immersed in dehydrated alcohol, is placed in baking oven (105 ℃), is dried to constant weight; Be placed in again retort furnace (temperature is 750 ℃) calcining 2.5h, cooling after taking out, weigh, calculate the aquation rate of product.
Embodiment 2:
With light magnesium oxide and water in mass ratio the 1:70 ratio mix, pour in there-necked flask ultra-sonic dispersion 30min under the 50Hz frequency into; Add subsequently the magnesium acetate that accounts for quality 5% and the polyoxyethylene glycol that accounts for quality 0.5%, be placed in 90 ℃ of waters bath with thermostatic control and stir, reaction 12h;
After reaction finishes, ultra-sonic dispersion after hydrated product is taken out, thin up, standing, suction filtration is immersed in dehydrated alcohol, is placed in baking oven (105 ℃), is dried to constant weight; Be placed in again retort furnace (temperature is 750 ℃) calcining 2.5h, cooling after taking out, weigh, calculate the aquation rate of product.
Embodiment 3:
With light magnesium oxide and water in mass ratio the 1:50 ratio mix, pour in there-necked flask ultra-sonic dispersion 30min under the 50Hz frequency into; Add subsequently the triethylenediamine that accounts for quality 3% and the spans that accounts for quality 0.2%, be placed in 50 ℃ of waters bath with thermostatic control and stir, reaction 8h;
After reaction finishes, ultra-sonic dispersion after hydrated product is taken out, thin up, standing, suction filtration is immersed in dehydrated alcohol, is placed in baking oven (105 ℃), is dried to constant weight; Be placed in again retort furnace (temperature is 750 ℃) calcining 2.5h, cooling after taking out, weigh, calculate the aquation rate of product.
Embodiment 4:
With light magnesium oxide and water in mass ratio the 1:60 ratio mix, pour in there-necked flask ultra-sonic dispersion 30min under the 50Hz frequency into; Add subsequently the vulkacit H that accounts for quality 1.0% and the Tweens that accounts for quality 0.3%, be placed in 80 ℃ of waters bath with thermostatic control and stir, reaction 10h;
After reaction finishes, ultra-sonic dispersion after hydrated product is taken out, thin up, standing, suction filtration is immersed in dehydrated alcohol, is placed in baking oven (105 ℃), is dried to constant weight; Be placed in again retort furnace (temperature is 750 ℃) calcining 2.5h, cooling after taking out, weigh, calculate the aquation rate of product.
Embodiment 5:
With light magnesium oxide and water in mass ratio the 1:30 ratio mix, pour in there-necked flask ultra-sonic dispersion 30min under the 50Hz frequency into; Add subsequently the magnesium acetate that accounts for quality 0.8% and the sucrose ester that accounts for quality 0.4%, be placed in 60 ℃ of waters bath with thermostatic control and stir, reaction 4h;
After reaction finishes, ultra-sonic dispersion after hydrated product is taken out, thin up, standing, suction filtration is immersed in dehydrated alcohol, is placed in baking oven (105 ℃), is dried to constant weight; Be placed in again retort furnace (temperature is 750 ℃) calcining 2.5h, cooling after taking out, weigh, calculate the aquation rate of product.
Embodiment 6:
With light magnesium oxide and water in mass ratio the 1:40 ratio mix, pour in there-necked flask ultra-sonic dispersion 30min under the 50Hz frequency into; Add subsequently the vulkacit H that accounts for quality 4.5% and the polyoxyethylene glycol that accounts for quality 0.35%, be placed in 70 ℃ of waters bath with thermostatic control and stir, reaction 6h;
After reaction finishes, ultra-sonic dispersion after hydrated product is taken out, thin up, standing, suction filtration is immersed in dehydrated alcohol, is placed in baking oven (105 ℃), is dried to constant weight; Be placed in again retort furnace (temperature is 750 ℃) calcining 2.5h, cooling after taking out, weigh, calculate the aquation rate of product.
Embodiment 7:
With light magnesium oxide and water in mass ratio the 1:35 ratio mix, pour in there-necked flask ultra-sonic dispersion 30min under the 50Hz frequency into; Add subsequently the triethylenediamine that accounts for quality 1.5% and the polyoxyethylene glycol that accounts for quality 0.08%, be placed in 55 ℃ of waters bath with thermostatic control and stir, reaction 3h;
After reaction finishes, ultra-sonic dispersion after hydrated product is taken out, thin up, standing, suction filtration is immersed in dehydrated alcohol, is placed in baking oven (105 ℃), is dried to constant weight; Be placed in again retort furnace (temperature is 750 ℃) calcining 2.5h, cooling after taking out, weigh, calculate the aquation rate of product.
Get the magnesium hydroxide 0.6g that produces under optimal conditions, be added in the 100ml dyeing waste water; The dispersion of mixed solution ultrasonic wave is rear with the first rapid stirring 5min of induction stirring, then low rate mixing 10min; Get supernatant liquor after sedimentation 1h and measure its colourity, calculate its percent of decolourization.Chroma removal rate through the magnesium hydroxide processed waste water reaches 96%.
Get the magnesium hydroxide 0.8g that produces under optimal conditions, be added in the 100ml dyeing waste water; The dispersion of mixed solution ultrasonic wave is rear with the first rapid stirring 5min of induction stirring, then low rate mixing 10min; Get supernatant liquor after sedimentation 1h and measure its colourity, calculate its percent of decolourization.The chroma removal rate of waste water reaches 98% after treatment.
Claims (7)
1. environmental protection level magnesium hydroxide production method, it is characterized in that: the industrial magnesium oxide that it is 1:20～1:70 that described method comprises mass ratio mixes with water, ultra-sonic dispersion 30min under the 50Hz frequency, then add the catalyzer that accounts for quality 0.5%～5% and the dispersion agent that accounts for quality 0.05%～0.5%, solution is placed in water bath with thermostatic control to be stirred, react 2h～12h at the temperature of 40 ℃～90 ℃, reaction finishes by standing, suction filtration, be dried to constant weight, product is immersed in dehydrated alcohol, again be dried to constant weight, then product is placed in retort furnace, 750 ℃ of calcining 1～5h, cooling getting final product after taking out.
2. a kind of environmental protection level magnesium hydroxide production method according to claim 1 is characterized in that: described catalyzer is for at least a in ammonium formiate, magnesium acetate, triethylenediamine, vulkacit H.
3. a kind of environmental protection level magnesium hydroxide production method according to claim 1, it is characterized in that: described dispersion agent is that a class is the polyalcohols material.
4. a kind of environmental protection level magnesium hydroxide production method according to claim 3, it is characterized in that: a described class is that the polyalcohols material is sucrose ester, polyoxyethylene glycol, spans or Tweens.
5. a kind of environmental protection level magnesium hydroxide production method according to claim 1, it is characterized in that: described industrial magnesium oxide is light magnesium oxide, has better activity, can be obtained by the magnesite calcining.
6. a kind of environmental protection level magnesium hydroxide production method according to claim 1, it is characterized in that: the magnesium hydroxide purity of preparation is high, granularity is little, specific surface area is large, the adsorption-flocculation ability is good, and all kinds of water pollutant matter are had good treatment effect.
7. a kind of environmental protection level magnesium hydroxide production method according to claim 1, it is characterized in that: products obtained therefrom is applied to the reactive black treatment of dyeing wastewater, and percent of decolourization is all more than 95%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111763116A (en) * | 2020-07-13 | 2020-10-13 | 广西南宁华夏农业科技有限公司 | Organic-inorganic compound fertilizer capable of adjusting acid, supplementing magnesium and preventing plant yellowing and preparation method thereof |
| CN112591774A (en) * | 2020-11-18 | 2021-04-02 | 潍坊凯博镁盐有限公司 | Method for preparing magnesium hydroxide by dry method |
| CN113979455A (en) * | 2021-11-10 | 2022-01-28 | 大连交通大学 | Preparation method and application of flaky superfine magnesium hydroxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10120416A (en) * | 1996-10-17 | 1998-05-12 | Kyowa Chem Ind Co Ltd | Magnesium hydroxide powder for aqueous suspension |
| CN101125669A (en) * | 2007-07-13 | 2008-02-20 | 马敬环 | Method for producing high-pure ultra-thin micro-powder magnesium hydroxide by extracting sea water |
| CN101269827A (en) * | 2008-04-02 | 2008-09-24 | 浙江工业大学 | Method for preparing high-dispersion magnesium hydroxide combustion inhibitor with one-step hydrothermal method |
| CN101318672A (en) * | 2008-07-09 | 2008-12-10 | 中国科学院青海盐湖研究所 | Method for preparing magnesium hydroxide with catalysis hydration of organic acid ammonium salts |
-
2011
- 2011-12-08 CN CN2011104046937A patent/CN103159236A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10120416A (en) * | 1996-10-17 | 1998-05-12 | Kyowa Chem Ind Co Ltd | Magnesium hydroxide powder for aqueous suspension |
| CN101125669A (en) * | 2007-07-13 | 2008-02-20 | 马敬环 | Method for producing high-pure ultra-thin micro-powder magnesium hydroxide by extracting sea water |
| CN101269827A (en) * | 2008-04-02 | 2008-09-24 | 浙江工业大学 | Method for preparing high-dispersion magnesium hydroxide combustion inhibitor with one-step hydrothermal method |
| CN101318672A (en) * | 2008-07-09 | 2008-12-10 | 中国科学院青海盐湖研究所 | Method for preparing magnesium hydroxide with catalysis hydration of organic acid ammonium salts |
Non-Patent Citations (2)
| Title |
|---|
| 孙永明等: "分散剂对制备超细氢氧化镁影响的实验研究", 《非金属矿》 * |
| 钱海燕等: "碱性溶液中氧化镁水化合成氢氧化镁颗粒", 《材料导报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111763116A (en) * | 2020-07-13 | 2020-10-13 | 广西南宁华夏农业科技有限公司 | Organic-inorganic compound fertilizer capable of adjusting acid, supplementing magnesium and preventing plant yellowing and preparation method thereof |
| CN112591774A (en) * | 2020-11-18 | 2021-04-02 | 潍坊凯博镁盐有限公司 | Method for preparing magnesium hydroxide by dry method |
| CN113979455A (en) * | 2021-11-10 | 2022-01-28 | 大连交通大学 | Preparation method and application of flaky superfine magnesium hydroxide |
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Application publication date: 20130619 |