CN111426635A - Method for detecting conversion rate of magnesium oxide to magnesium hydroxide - Google Patents
Method for detecting conversion rate of magnesium oxide to magnesium hydroxide Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 69
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 65
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 64
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 64
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 58
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 50
- 238000012360 testing method Methods 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000004364 calculation method Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 238000001291 vacuum drying Methods 0.000 claims abstract description 5
- 238000005070 sampling Methods 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 8
- 238000004458 analytical method Methods 0.000 claims description 4
- 238000011065 in-situ storage Methods 0.000 claims 2
- 238000001514 detection method Methods 0.000 abstract description 5
- 238000006703 hydration reaction Methods 0.000 description 28
- 230000036571 hydration Effects 0.000 description 26
- 239000000047 product Substances 0.000 description 19
- 239000000523 sample Substances 0.000 description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 230000008569 process Effects 0.000 description 11
- 238000005979 thermal decomposition reaction Methods 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 6
- 229910052749 magnesium Inorganic materials 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000001095 magnesium carbonate Substances 0.000 description 5
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 5
- 235000014380 magnesium carbonate Nutrition 0.000 description 5
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 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 description 4
- 229910052599 brucite Inorganic materials 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 239000003063 flame retardant Substances 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 3
- 239000000920 calcium hydroxide Substances 0.000 description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 235000010755 mineral Nutrition 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000004445 quantitative analysis Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 159000000003 magnesium salts Chemical class 0.000 description 2
- 239000008267 milk Substances 0.000 description 2
- 210000004080 milk Anatomy 0.000 description 2
- 235000013336 milk Nutrition 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000000887 hydrating effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000009659 non-destructive testing Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a method for detecting the conversion rate of magnesium oxide to magnesium hydroxide, which comprises the following steps of (1) preparing a standard sample, mixing raw materials of magnesium oxide and standard magnesium hydroxide by adopting absolute ethyl alcohol as a solvent, stirring, filtering, vacuum-drying to obtain a batch of mixed standard samples with different magnesium hydroxide contents, and calculating the conversion rate of the mixed standard samples, (2) performing color difference detection on the mixed standard samples by adopting a color difference meter to obtain a group of L, a and b, (3) obtaining whiteness according to a whiteness calculation formula on the data, and (4) performing linear fitting on the whiteness and the conversion rate of the mixed standard samples to obtain a linear fitting equation, and (5) during detection, randomly sampling on site, testing and calculating the whiteness by adopting the color difference meter, and substituting the linear fitting equation to obtain the conversion rate.
Description
Technical Field
The invention relates to a material detection technology, in particular to a method for detecting the conversion rate of magnesium oxide to magnesium hydroxide.
Background
The magnesium hydroxide is used as an important chemical product and an intermediate, and has wide application in the fields of ceramic materials, environmental protection, medicines and the like. The method has the advantages that the consumption is high, and the using effect is obvious, and the method is mainly applied to three fields: the flame retardant is used as an inorganic additive type nontoxic flame retardant and has various performances of flame retardance, smoke abatement, dripping resistance, filling and the like; secondly, the method can be used for wastewater treatment and flue gas desulfurization in the environmental field; thirdly, the high-purity magnesium hydroxide is one of the most important raw materials for producing the high-purity magnesium oxide. The preparation of magnesium hydroxide starts in the 30 s of the 20 th century, and a plurality of preparation methods are developed for more than 80 years and mainly divided into a physical crushing method and a chemical synthesis method.
The physical grinding method is to directly grind the ore, and prepare the magnesium hydroxide product with the required granularity grade by dry coarse grinding and wet ultrafine grinding, wherein the more commonly used ore is brucite. The natural mineral crushing method has the advantages of wide source of brucite as a raw material, low cost, simple operation process and less environmental pollution. However, the ore particles are large, ultra-fining treatment is required, and the development of the ore is limited, and moreover, the high-quality brucite reserves cannot meet the increasing demand, so that the chemical synthesis method becomes the mainstream. The method is generally to prepare a magnesium-containing raw material by a reaction conversion method, wherein the commonly used magnesium-containing raw material mainly comprises magnesite, serpentine, dolomite, brucite, seawater, brine, halogen sheets, bromine preparation waste liquid, magnesium sulfate and the like, and the magnesium-containing raw material is specifically divided into two categories: the other method is to process magnesium oxide from magnesium-containing mineral, then hydrate light magnesium oxide to obtain magnesium hydroxide, which belongs to hydration method, and the reaction mechanism is as follows:
MgO+H2O→Mg(OH)2
the other is prepared by precipitating brine or soluble magnesium salt and alkali substances, belongs to a liquid-phase precipitation method, and has the following reaction mechanism:
Mg2++2OH-→Mg(OH)2
according to the above OH-The difference in the source can be divided into an ammonia process, a calcium hydroxide process (lime milk process) and a sodium hydroxide process in actual production and development. (1) The ammonia process is a method which is adopted in actual production more often because the ammonia water is weak base, NH4+The solubility of the magnesium hydroxide can be increased, the supersaturation degree of the system is reduced, and the reaction process and the appearance and the particle size of the magnesium hydroxide product are easy to control. When the ammonia method is adopted for production, the yield of the product is low, and the operation environment is poor because the ammonia water is easy to volatilize. (2) The calcium hydroxide in the calcium hydroxide method (lime milk method) is cheap and easy to obtain, so the method has higher industrial application value. But the product has small granularity, large agglomeration tendency, extremely difficult filtration and easy adsorption of impurity ions such as silicon, magnesium, calcium, iron and the like, onlyThe method is suitable for industries with low requirement on purity, such as flue gas desulfurization, waste water neutralization and the like, and the method is not generally used for preparing high-purity magnesium hydroxide. And the method produces a large amount of CaCl2The formation of by-products, if not effectively utilized, results in the accumulation of new waste, rendering the scale of production impossible to expand. (3) The sodium hydroxide method is to react magnesium salt with sodium hydroxide to prepare magnesium hydroxide, and the prepared product has high purity, uniform particle size and regular shape, and is attracting wide attention of people. However, sodium hydroxide is strong alkali, the reaction process is rapid, the generated magnesium hydroxide forms colloidal precipitate due to the generation of a large amount of new nuclei, the product often has small particle size, is extremely difficult to settle and filter, and is easy to carry more sodium ions and chloride ions, so the method has strict synthesis conditions. In short, the liquid phase precipitation method is harsh to the reaction conditions, and requires investment in environmental protection equipment and subsequent treatment of reaction by-products. The hydration method calcines the ore, and the magnesium hydroxide is prepared by hydrating the prepared magnesium oxide, which is a process of magnesium oxide dissolution and magnesium hydroxide precipitation. In this field, many researchers and enterprises have made many practices for the development and production of magnesium hydroxide from magnesium oxide.
Sunyongming et al, Nanjing Industrial university, in the Experimental research on the influence of a dispersant on the preparation of ultrafine magnesium hydroxide (nonmetallic ore, volume 28, No. 4, 7 months 2005), proposed the hydration preparation of ultrafine magnesium hydroxide from magnesium oxide calcined from magnesite. Adding the dispersing agent after the hydration reaction is carried out for a period of time, and investigating the influence of the type and the dosage of the dispersing agent on the size of the magnesium hydroxide particles; sunyongming of Nanjing Industrial university, Suoshi graduate, the thesis of magnesite calcined magnesia hydrated to prepare high-purity superfine magnesium hydroxide, proposes that the filtered product is dried at 105 ℃, weighed accurately after being dried completely, then calcined at 500 ℃ for 2.0h to completely decompose magnesium hydroxide, taken out, cooled and weighed, and then the hydration rate of magnesium oxide is calculated. By the following formula:
in the formula: m is1-weight before calcination after the hydration product has been completely dried; m is2-the weight of the hydrated product after calcination.
The relation between the hydration degree and the hydration time of light-burned magnesium oxide samples at different temperatures and magnesium oxide in an alkaline solution at 70 ℃ is researched by Haimai, et al, Nanjing university of Industrial science, in the kinetics of hydration of light-burned magnesium oxide (chemical minerals and processing, 2007, 12 th). Wherein the hydration degree of magnesium oxide is calculated according to the above formula (1). The study on the preparation of light-burned magnesium oxide from magnesite and the hydration kinetics thereof published by Liuxin Wei of Beijing university of science and technology and the like (journal of the university of China (Nature science edition), 2011, volume 42, phase 12) proposes: the method is characterized in that magnesite is used as a raw material to prepare light-burned magnesium oxide, the hydration kinetics of the light-burned magnesium oxide is researched, and the influence of the hydration temperature, the mass concentration and the granularity of the magnesium oxide on the hydration process is examined. Meanwhile, the method for calcining the dried hydration product at 500 ℃ for 2 hours to calculate the conversion rate of the hydration product is given, and the calculation formula is basically according to the formula (1). In the research on flame retardant grade magnesium hydroxide prepared by magnesium oxide hydration method, a university of Tianjin technology, Wang Lisha Master, 2013, "the hydration rate of magnesium oxide can be obtained by burning the dried product and obtaining the hydration rate of magnesium oxide from the poor quality before and after burning", and the calculation formula is as shown in the formula (1). In the research on preparation of magnesium hydroxide by hydration of magnesium oxide (salt industry and chemical industry, 3 months 2012, volume 41, phase 3), chenxian et al, tianjin science and technology university, experimental research on preparation of magnesium hydroxide by hydration using magnesium oxide prepared by pyrolysis of bischofite as a raw material was carried out. Through single factor test and orthogonal test, the influence of reaction time, reaction temperature, liquid-solid ratio and stirring speed on the hydration rate of the magnesium oxide is investigated, the hydration reaction condition is optimized, and the hydration rate calculation formula also adopts the formula (1).
The relative mass X of magnesium oxide is provided by the principle of quantitative analysis of the phase of ray diffraction in the Master thesis of Limei of northeast university (2005) of hydration method for preparing flame retardant grade magnesium hydroxideMgOThe smaller the content, the higher the MgO conversion rate, the smaller the formula:
in the formula: i is(002)MgOThe diffraction intensity of the magnesium oxide is the integral intensity of the diffraction line corresponding to the (002) crystal face of the magnesium oxide; i is(101)Mg(OH)2The diffraction intensity of magnesium hydroxide is the integrated intensity of the diffraction line corresponding to the crystal face of magnesium hydroxide (101). In the research on magnesium hydroxide preparation from magnesium oxide in salt lake (metal mine, No. 7 of 2007, No. 373), the university of northeast China, Yiwanloyal et al, proposed that the comprehensive utilization of salt lake resources is taken as background, magnesium oxide products in certain salt lake in Qinghai are taken as raw materials, and the technological conditions for preparing magnesium hydroxide by adopting a hydration method are researched; the influence rule of reaction parameters such as reaction temperature, reaction time, solid-liquid ratio of raw materials and the like on the conversion rate of the raw materials and the particle size of a product is researched through a single-factor condition test, and the preparation mechanism of preparing magnesium hydroxide by a magnesium oxide hydration method is explored. Calculating the relative mass X of magnesium oxide of the product according to the X-ray diffraction dataMgOThe calculation formula follows the above formula (2).
The two test methods, one of the formula (1) thermal decomposition method requires the muffle furnace to be calcined to 600 ℃ and needs to consume more time and energy; the other formula (2) is an X-ray diffraction method, an X-ray diffractometer is needed, sample preparation, test and analysis are carried out, and the cost is high. The quality control brought by the sample conversion rate (hydration rate) in the industry becomes a difficult problem, and the quality of products in the industry and the utilization of later-stage products are seriously influenced.
Disclosure of Invention
The existing X-ray diffraction method relates to expensive and complex test equipment, has radioactive radiation and needs a professional person to operate; the thermal decomposition method consumes time and energy, and the method for detecting the conversion rate of magnesium oxide to magnesium hydroxide has the advantages of no need of consumables, low cost of a test instrument, good environment and testers, simple and quick test speed, capability of realizing industrial Internet and the like.
In order to achieve the purpose, the method comprises the steps of establishing a linear relation between whiteness and conversion rate (magnesium hydroxide content) through the color difference of magnesium oxide and magnesium hydroxide, particularly the whiteness difference caused after mixing, and calculating the conversion rate through testing the color difference of a sample.
The invention aims to realize the following technical scheme that the method for detecting the conversion rate of magnesium oxide into magnesium hydroxide comprises the following steps: (1) preparing a standard sample, mixing the raw material magnesium oxide and standard magnesium hydroxide according to different mass proportions, stirring for 15-30min by adopting absolute ethyl alcohol as a solvent during mixing, filtering, and carrying out vacuum drying at 60-80 ℃ for 0.5-3h to obtain a batch of magnesium hydroxide with the content XiUnequal mixed standards, calculating the conversion rate y of the mixed standardsiDetecting color difference of the standard sample, and performing color difference analysis operation on the mixed standard samples by using a color difference meter to obtain a group of Li(lightness) ai(red green color range value) and bi(yellow-blue range values) data; (3) calculating the whiteness of the standard sample, and obtaining the whiteness W according to the whiteness calculation formula on the data setiA numerical value; (4) fitting linear equation to whiteness W of mixed standard sampleiNumber and conversion yiCarrying out linear fitting to obtain a linear fitting equation of whiteness W and conversion rate y, (5) carrying out field test, randomly sampling in the field, and measuring a sample to be detected L by using a color difference metern、anAnd bnCalculating WnW is to benSubstituting the linear fitting equation to calculate the conversion rate yn。
The above-mentioned standard magnesium hydroxide is commercially available, and is required to have a purity of 99.0% or more, an average particle diameter of 50 μm and a bulk density of 1.29g/cm3The purchasing trade company has the Qinghai West magnesium industry, Merck (China), Aladdin reagent and the like.
Preferably, when the raw material magnesium oxide and the standard magnesium hydroxide are mixed, absolute ethyl alcohol is used as a solvent, stirring is carried out for 20min, filtering is carried out, and vacuum drying is carried out for 2h at 70 ℃ to obtain a mixed standard sample.
Preferably, the mass ratio of the raw material magnesium oxide to the standard magnesium hydroxide is as follows: 0: 10; 1: 9; 2: 8; 3: 7; 4: 6; 5: 5; 6: 4; 7: 3; 8: 2; 9: 1; 10:0, corresponding to a conversion of magnesium hydroxide of from 100%; 86.12 percent; 73.39 percent; 61.67 percent; 50.85 percent; 40.82 percent; 31.50 percent; 22.81 percent; 14.71 percent; 7.12 percent; 0.
the whiteness degree calculation formula is as follows:
the gain effect of the invention is as follows:
1. the method for detecting the conversion rate of magnesium oxide to magnesium hydroxide is different from the conventional X-ray diffraction method and thermal decomposition method, greatly reduces the sample test cost, the personnel test operation difficulty and the test time period cost, and is beneficial to the development of the magnesium hydroxide industry;
2. the method for detecting the conversion rate of magnesium oxide to magnesium hydroxide directly adopts the optical chromatic aberration principle to obtain test data, the artificial interference and the operation error in the whole process are greatly reduced, the manual reference determination is needed compared with the integration of an X-ray diffraction method, and the weighing is more reliable when the thermal decomposition method needs higher temperature;
3. the method for detecting the conversion rate of magnesium oxide to magnesium hydroxide can ensure a faster experimental result, is very favorable for field detection, and creates possibility for the next industrial internet if a signal of a probe of a color difference meter can be directly connected with an MES system;
4. the method for detecting the conversion rate of magnesium oxide to magnesium hydroxide has the advantages of simple and quick whole detection process, good repeatability, suitability for testing large-batch samples and wide application range.
5. The method for detecting the conversion rate of magnesium oxide into magnesium hydroxide belongs to the fields of nondestructive testing and optics in terms of mechanism, and is also suitable for detecting the conversion rate of magnesium oxide into magnesium hydroxide.
Drawings
FIG. 1 is a graph of whiteness versus conversion for a mixed standard. Wherein the straight line is a linear fitting curve, WiRepresents the whiteness value, yiRepresenting the conversion of magnesium oxide to magnesium hydroxide.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Firstly, preparing a standard sample, mixing raw material magnesium oxide and standard magnesium hydroxide according to different mass proportions, stirring for 20min by adopting absolute ethyl alcohol as a solvent during mixing, filtering, and carrying out vacuum drying for 2h at 70 ℃ to obtain a batch of magnesium hydroxide content XiAnd (4) calculating the conversion rate yi of the mixed standard samples according to the unequal mixed standard samples. The mass ratio of the raw material magnesium oxide to the standard magnesium hydroxide is as follows: 0: 10; 1: 9; 2: 8; 3: 7; 4: 6; 5: 5; 6: 4; 7: 3; 8: 2; 9: 1; 10:0, corresponding to a conversion of magnesium hydroxide of from 100%; 86.12 percent; 73.39 percent; 61.67 percent; 50.85 percent; 40.82 percent; 31.50 percent; 22.81 percent; 14.71 percent; 7.12 percent; 0, shown in table 1 below.
Secondly, detecting the color difference of the standard sample, and performing color difference analysis operation on the 10 mixed standard samples by using a precision color difference meter HP-200 (handheld type) to obtain a group of Li(lightness) ai(red green color range value) and bi(yellow-blue range values) data, shown in table 1 below.
Thirdly, calculating the whiteness of the standard sample, calculating 10 groups of data of a color difference meter, and obtaining the whiteness WiNumerical values. According to a whiteness calculation formula:
the correlation calculation results are also shown in table 1. Wherein, the 1# sample, standard magnesium hydroxide 100% is used as a standard white sheet and is determined as whiteness 100.
TABLE 1 data relating to the standard samples according to the invention
(precision colorimeter HP-200 (hand-held), equipment supplier Schchen Tai run-Union science and technology development Co., Ltd.)
| Reference numerals | MMgO:MMg(OH)2 | Xi％ | yi | Li | ai | bi | Wi％ |
| 1# | 0:10 | 100 | 1 | - | - | - | 100 |
| 2# | 1:9 | 90 | 0.8612 | 99.79 | -0.39 | -0.19 | 99.52 |
| 3# | 2:8 | 80 | 0.7339 | 99.68 | -0.70 | 0.40 | 99.13 |
| 4# | 3:7 | 70 | 0.6167 | 99.46 | -0.77 | 0.69 | 98.83 |
| 5# | 4:6 | 60 | 0.5085 | 99.13 | -0.79 | 0.93 | 98.50 |
| 6# | 5:5 | 50 | 0.4082 | 99.12 | -0.80 | 1.32 | 98.22 |
| 7# | 6:4 | 40 | 0.315 | 98.94 | -1.16 | 1.30 | 97.96 |
| 8# | 7:3 | 30 | 0.2281 | 98.57 | 0.77 | 1.76 | 97.61 |
| 9# | 8:2 | 20 | 0.1471 | 98.19 | 0.61 | 1.66 | 97.47 |
| 10# | 9:1 | 10 | 0.0712 | 98.15 | -0.84 | 2.00 | 97.15 |
| 11# | 10:0 | 0 | 0 | 98.06 | 1.50 | 1.84 | 96.93 |
The fourth step is to fit a linear equation to obtain the whiteness WiAnd conversion yiAnd (3) performing linear fitting to obtain a linear fitting straight line as shown in FIG. 1, wherein the equation is as follows:
Wi＝3.0077yi+96.965-----------------------------(4)
in the formula: wiAs whiteness of the sample, yiConversion of magnesium oxide to magnesium hydroxide, R2When 0.9985, the above equation is transformed to:
and finally, performing field test, detecting the whiteness of 3 commercially available actual samples, calculating by formulas (3) and (5) to obtain a result, and comparing a calculation result K of an XRD diffraction quantitative method with a thermal decomposition method M and a test result list 2. The conversion standard deviation value S obtained by the testing method is smaller than that obtained by an XRD quantitative method and a thermal decomposition method, the deviation degree is smaller, the dispersion degree is smaller, and the reliability is higher. The reason may be that the XRD quantification method involves integral calculation, and there is an operation of manually performing baseline adjustment; the thermal decomposition method has sampling error of the sample, is closely related to the humidity on the surface of the sample, and is easy to absorb moisture to influence the quality of the sample. Therefore, the method has higher accuracy in the aspect of data reliability.
TABLE 2 conversion of the commercial products three test results
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and those skilled in the art can make various modifications and changes, such as conversion calculation of mass percent of a certain component. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. A method for detecting the conversion rate of magnesium oxide into magnesium hydroxide is characterized by comprising the following steps:
(1) preparation of Standard samples
Mixing raw material magnesium oxide and standard magnesium hydroxide according to different mass proportions, stirring for 15-30min by using absolute ethyl alcohol as a solvent during mixing, filtering, and vacuum drying at 60-80 ℃ for 0.5-3h to obtain a batch of magnesium hydroxide content XiUnequal mixed standards, calculating the conversion rate y of the mixed standardsi；
(2) Detecting color difference of standard sample
Performing color difference analysis on the mixed standard samples by using a color difference meter to obtain a group of Li(lightness) ai(red green color range value) and bi(yellow-blue range values) data;
(3) calculating standard sample whiteness
Obtaining the whiteness W according to the whiteness calculation formula on the data setiA numerical value;
(4) fitting linear equation
Whiteness W to mixed standardsiNumber and conversion yiPerforming linear fitting to obtain a linear fitting equation of whiteness W and conversion rate y;
(5) in situ testing
Randomly sampling in situ, and measuring L sample to be detected by color difference metern、anAnd bnComputingWnW is to benSubstituting the linear fitting equation to calculate the conversion rate yn。
2. The method for detecting the conversion rate of magnesium oxide into magnesium hydroxide according to claim 1, wherein: the standard magnesium hydroxide has a purity of 99.0% or more, an average particle diameter of 50 μm, and a bulk density of 1.29g/cm3。
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