CN104777064A - Method for measuring silicon dioxide content in refractory materials - Google Patents
Method for measuring silicon dioxide content in refractory materials Download PDFInfo
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- CN104777064A CN104777064A CN201510112737.7A CN201510112737A CN104777064A CN 104777064 A CN104777064 A CN 104777064A CN 201510112737 A CN201510112737 A CN 201510112737A CN 104777064 A CN104777064 A CN 104777064A
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Abstract
The invention discloses a method for measuring the silicon dioxide content in refractory materials, and aims to provide a method that can safely and efficiently measure the silicon dioxide content in refractory materials. The method comprises the following steps: adding a blank sample and a sample with a mass (m) into a mixed solvent of waterless sodium carbonate and boric acid according to a mass ratio of 2:1, melting the blank sample and sample at a high temperature; extracting by diluted hydrochloric acid to prepare solutions, condensing the solutions to obtain wet-salt liked substances; adding a polyoxyethylene water solution, evenly stirring, adding hot water to dissolve, filtering, washing the precipitates, washing the precipitates by hot hydrochloric acid for 7 to 8 times, then washing the precipitates by hot water for 9 to 10 times, burning the precipitates in a muffle furnace, cooling, weighing to obtain the blank sample precipitate weight (m0) and the sample precipitate weight (m1), and calculating the SiO2 content according to the following formula: WSiO2=100%(m1-m0)/m, wherein the m0 represents the blank sample precipitate weight, the m1 represents the sample precipitate weight, m represents the sample weight, and the measurement unit of m, m0, and m1 is g.
Description
Technical field
The present invention relates to technical field of refractory materials, particularly relate to the method for dioxide-containing silica in a kind of novel precipitation agent polyoxyethylene gravimetric determination fire resistive material.
Background technology
Fire resistive material, in the industry such as metallurgy, silicate, chemical industry, power, oil, machine-building, is used widely.In ferrous metallurgical industry, coke oven is mainly made up of fire resistive material, the blast furnace of steel-making and heat generator, and the inequality such as various converter, soaking pit, heating furnace be unable to do without various fire resistive material.Not only the die casting of molten steel will consume a large amount of fire resistive materials, and continuous casting more needs the fire resistive material of some high-qualitys, and external refining does not have the fire resistive material of fine quality to have no way of realizing yet.Fire resistive material is the basic material of serving high-temperature technology, it is the structured material of building the Thermal Equipments such as high temperature kiln by laying bricks or stones, fire resistive material is mainly used in metallurgical industry, it is the important foundation of metallurgical industry development, in recent years along with the increase fire resistive material consumption of output of steel also constantly increases, and as the indispensable raw material of fire resistive material, high-aluminium vanadine demand also constantly to increase and essential.All containing more silicon dioxide in fire resistive material, silicon dioxide is at high temperature acid, silica refractory energy resistance to acid slag corrosion.
The rauhkalk series fire resistive material of high-quality has the ability of very strong alkali resistance scouring and good creep properties, be widely used in cement kiln, converter, electric furnace, steel-making, continuous casting production, refining furnace, particularly in Clean Steel Smelting, special steel, play an important role.All containing more silicon dioxide in fire resistive material, silicon dioxide is at high temperature acid, silica refractory energy resistance to acid slag corrosion.Therefore in fire resistive material, the mensuration of silicon dioxide is particularly important, is one of leading indicator evaluating fire resistive material quality, is also the main authority that fire resistive material enters that factory's quality is checked on and price is settled accounts.
The method of silicon dioxide mainly perchloric acid determination and colourimetry in current mensuration fire resistive material, national standard is also perchloric acid determination.Although perchloric acid is desirable precipitation agent, the exhausting cabinet of Long-Time Service perchloric acid and air draft pipe, easily cause burning and blast, dangerous property, be therefore badly in need of the method for dioxide-containing silica in a kind of mensuration fire resistive material newly of research and development.
Summary of the invention
The technical problem to be solved in the present invention is to provide the method for dioxide-containing silica in a kind of safe, efficient mensuration fire resistive material.
For reaching above-mentioned purpose, the assay method of dioxide-containing silica in a kind of fire resistive material of the present invention, comprises the following steps:
1) not add the blank test of sample and to add the melting under the mixed solvent high temperature of natrium carbonicum calcinatum and boric acid 2:1 of sample that quality is m;
2) extract, after being processed into solution, after test solution being concentrated into wet salt shape with watery hydrochloric acid;
3) add polyoxyethylene aqueous solution to stir, heating water dissolves, and filters, washing precipitation, with hot salt pickling precipitation 7-8 time, then with hot water wash precipitation 9-10 time, will precipitate as calcination in muffle furnace, cooling, weigh, blank test and specimen test are respectively m0 and m1;
W
SiO2＝100％(m1－mo)/m
In formula: mo: be blank precipitation quality, g;
M1: be sample precipitation quality, g;
M: sample mass, g.
Wherein said sample is through mixed solvent melting 30-50min in 850-900 DEG C of muffle furnace.
Wherein said step 2) in the concentration of watery hydrochloric acid be 50%.
Wherein said polyoxyethylene concentration of aqueous solution is 2g/L.
Wherein said step 3) in hot water temperature be 70 ~ 80 DEG C.
Wherein said step 3) in muffle furnace 900 DEG C of calcination 40min.
Wherein said step 3) in hot concentration of hydrochloric acid be 5%, temperature is 100 DEG C, and hot water temperature is 100 DEG C.
The invention difference from existing technology is that the present invention achieves following technique effect:
1) the inventive method is suitable with the accuracy of perchloric acid determination, although perchloric acid is desirable precipitation agent, but the exhausting cabinet of Long-Time Service perchloric acid and air draft pipe easily cause burning or blast, use novel precipitation agent polyoxyethylene to reduce the danger in operating, but security promote greatly;
2) in the inventive method mensuration fire resistive material, the content cost of silicon dioxide reduces greatly:
Perchloric acid determination: each sample of primary dewatering (single sample) perchloric acid used is 15-60ml in analytic process, the cost of perchloric acid is about 1.1-4.3 unit (current perchloric acid price 36 yuan/bottle (A.R)).
Polyoxyethylene gravimetric method: each sample of primary dewatering (single sample) polyoxyethylene used is 10ml (2g/L) in analytic process, the cost of polyoxyethylene is about 0.5 point (0.1 yuan/g), lower than the cost of perchloric acid 300-864 times.
Embodiment
Below in conjunction with embodiment, to above-mentioned being described in more detail with other technical characteristic and advantage of the present invention.
1. method summary:
Sample is through mixed solvent melting, extract, after being processed into solution, after test solution being concentrated into wet salt shape with watery hydrochloric acid, add 7-8ml polyoxyethylene (2g/L), stir, add 50ml hot water (70 ~ 80 DEG C) dissolved salts, filter, washing precipitation, to precipitate as calcination in muffle furnace, cooling, weighs.
2: reagent:
2.1: hydrochloric acid
2.2 mixed solvents (two parts of natrium carbonicum calcinatums and the mixing of a boric acid)
2.3 polyethylene oxide solutions (2g/L): take 0.2g polyoxyethylene, add 100ml water, stirring and dissolving (used time now joins)
3: sampling and sample preparation: Q/BGJH-01-04-2008 carry out sample manufacture
4: sample size: take sample 0.2500g
5: blank: blank with batch band
The platinum crucible of 2.5-3g mixed solvent will be mixed with in advance, melting about 40min in 850-900 DEG C of muffle furnace, take out cooling, put into 400mL beaker, add 50mL hydrochloric acid (50%)
Leaching frit, crucible is washed out with intermediate water, solution after leaching frit is concentrated into wet salt shape, with filter paper, glass bar and beaker sidewall are wiped clean, add 20mL polyethylene oxide solutions (2g/L), stir, with glass bar, caking is smashed to pieces, place 5-10min, add 50mL hot water (70-80 DEG C) dissolved salts, filter with middling speed quantitative filter paper, clean beaker, wash precipitation 8-9 time by heat (100 DEG C) hydrochloric acid (5%), then use hot water (100 DEG C) to wash precipitation 9-10 time.To precipitate and move in porcelain crucible together with filter paper, carbonization, ashing, at 900 DEG C of calcination 40min, take out, be chilled to room temperature, weigh, calcination is to constant weight repeatedly, and quality is mo.
6: analytical procedure:
The sample 0.2500g taken is placed in the platinum crucible being mixed with 2.5-3g mixed solvent in advance, mix with glass bar, and be placed on surface with a small amount of mixed solvent, melting about 40min in 850-900 DEG C of muffle furnace, take out cooling, put into 400mL beaker, add 50mL hydrochloric acid (50%) leaching frit, crucible is washed out with intermediate water, solution after leaching frit is concentrated into wet salt shape, with filter paper, glass bar and beaker sidewall are wiped clean, add 20mL polyethylene oxide solutions (2g/L), stir, with glass bar, caking is smashed to pieces, place 5-10min, add 50mL hot water (70-80 DEG C) dissolved salts, filter with middling speed quantitative filter paper, clean beaker, precipitation 8-9 time is washed by heat (100 DEG C) hydrochloric acid (5%), then hot water (100 DEG C) is used to wash precipitation 9-10 time, to precipitate and move in porcelain crucible together with filter paper, carbonization, ashing, at 900 DEG C of calcination 40min, take out, be chilled to room temperature, weigh, calcination is to constant weight repeatedly, quality is m1.
7 results calculate:
W(SiO
2)(％)＝100(m1－mo)/m
In formula: mo: be blank precipitation quality (g)
M1: be sample precipitation quality (g)
M: sample mass (g)
8: accuracy and precision
Getting the samples such as silicon mark liquid, High-Alumina clay adopts the rare method of polyoxyethylene repeatedly to test, and test value is as shown in table 1, table 2 and table 3:
The mensuration of dioxide-containing silica in table 1 silicon mark liquid
The mensuration of dioxide-containing silica in table 2 High-Alumina clay
From table 1 and table 2: the method precision is good
The mensuration of dioxide-containing silica in No. 13, table 3 clay, open fire jewel 416 and lime stone
As can be seen from Table 3, the method accuracy is good
Get the silicon dioxide standard solution of two parts of identical amounts, do precipitation agent respectively with perchloric acid and polyoxyethylene, carry out silica weight method mensuration, measurement result sees the following form 4:
Table 4 does precipitation agent with perchloric acid and polyoxyethylene and carries out silica weight method measurement result
When table 4 illustrates that polyoxyethylene does precipitation agent, sedimentation effect is more equal to or slightly better than the sedimentation effect of perchloric acid dehydration (primary dewatering).
It is as shown in table 5 that the rare method of various sample polyoxyethylene and perchloric acid dewatering compare the data obtained.
The rare method of table 5 polyoxyethylene compares with perchloric acid dewatering
Analyze same sample by the method and perchloric acid dehydrated weight method as can be seen from Table 5, table 5 data show that the rare method of polyoxyethylene compares with perchloric acid dewatering, close with perchloric acid method's determination data.
The present invention measures silicon dioxide in fire resistive material by adopting the novel precipitation agent of polyoxyethylene, and accuracy and precision aspect and perchloric acid determination quite, are better than perchloric acid determination at analysis cost and security.Polyoxyethylene can replace perchloric acid as precipitation agent in gravimetric method.There is good economic benefit and social benefit.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (7)
1. the assay method of dioxide-containing silica in fire resistive material, is characterized in that comprising the following steps:
1) not add the blank test of sample and to add the melting under the mixed solvent high temperature of natrium carbonicum calcinatum and boric acid 2:1 of sample that quality is m;
2) extract, after being processed into solution, after test solution being concentrated into wet salt shape with watery hydrochloric acid;
3) add polyoxyethylene aqueous solution to stir, heating water dissolves, and filters, washing precipitation, with hot salt pickling precipitation 7-8 time, then with hot water wash precipitation 9-10 time, will precipitate as calcination in muffle furnace, cooling, weigh, blank test and specimen test are respectively m0 and m1;
W
SiO2＝100％(m1－mo)/m
In formula: mo: be blank precipitation quality, g;
M1: be sample precipitation quality, g;
M: sample mass, g.
2. the assay method of dioxide-containing silica in fire resistive material according to claim 1, is characterized in that: described sample is through mixed solvent melting 30-50min in 850-900 DEG C of muffle furnace.
3. the assay method of dioxide-containing silica in fire resistive material according to claim 1, is characterized in that: described step 2) in the concentration of watery hydrochloric acid be 50%.
4. the assay method of dioxide-containing silica in fire resistive material according to claim 1, is characterized in that: described polyoxyethylene concentration of aqueous solution is 2g/L.
5. the assay method of dioxide-containing silica in fire resistive material according to claim 1, is characterized in that: described step 3) in hot water temperature be 70 ~ 80 DEG C.
6. the assay method of dioxide-containing silica in fire resistive material according to claim 1, is characterized in that: described step 3) in muffle furnace 900 DEG C of calcination 40min.
7. the assay method of dioxide-containing silica in fire resistive material according to claim 1, is characterized in that: described step 3) in hot concentration of hydrochloric acid be 5%, temperature is 100 DEG C, and hot water temperature is 100 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106556615A (en) * | 2016-11-21 | 2017-04-05 | 厦门出入境检验检疫局检验检疫技术中心 | The detection method of silicon doping situation in a kind of iron scale |
| CN110146405A (en) * | 2019-06-05 | 2019-08-20 | 核工业北京地质研究院 | The measuring method of boron carbide mass fraction in a kind of aluminum-based boron carbide neutron absorber material |
| CN114088571A (en) * | 2021-11-08 | 2022-02-25 | 包头钢铁（集团）有限责任公司 | Method for measuring content of silicon dioxide in high-silicon composite flux |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106556615A (en) * | 2016-11-21 | 2017-04-05 | 厦门出入境检验检疫局检验检疫技术中心 | The detection method of silicon doping situation in a kind of iron scale |
| CN106556615B (en) * | 2016-11-21 | 2019-03-05 | 厦门出入境检验检疫局检验检疫技术中心 | The detection method of silicon doping situation in a kind of iron scale |
| CN110146405A (en) * | 2019-06-05 | 2019-08-20 | 核工业北京地质研究院 | The measuring method of boron carbide mass fraction in a kind of aluminum-based boron carbide neutron absorber material |
| CN114088571A (en) * | 2021-11-08 | 2022-02-25 | 包头钢铁（集团）有限责任公司 | Method for measuring content of silicon dioxide in high-silicon composite flux |
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