CN108489849A - The method and alumina product grade discrimination of boron are quickly detected in Alpha-alumina - Google Patents

The method and alumina product grade discrimination of boron are quickly detected in Alpha-alumina Download PDF

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Publication number
CN108489849A
CN108489849A CN201810157667.0A CN201810157667A CN108489849A CN 108489849 A CN108489849 A CN 108489849A CN 201810157667 A CN201810157667 A CN 201810157667A CN 108489849 A CN108489849 A CN 108489849A
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Prior art keywords
alumina
product
boron
alpha
beaker
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CN201810157667.0A
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CN108489849B (en
Inventor
张冬梅
王霄楠
李民菁
邵梅珊
李莉真
马春玲
满俊艳
王双丽
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HENAN CHANGXING INDUSTRY Co Ltd
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HENAN CHANGXING INDUSTRY Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G01N5/04Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38Diluting, dispersing or mixing samples
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38Diluting, dispersing or mixing samples
    • G01N2001/386Other diluting or mixing processes

Abstract

The method and alumina product grade discrimination of boron are quickly detected in alpha-aluminium oxide, provide a kind of method reacted with polyvinyl alcohol by alpha-aluminium oxide quickly to detect the boron content in aluminium oxide, and the technique that the grade of alumina product is judged with this, it by sampling, dispensing, gelling, dumping tower tray, weighs, calculate, compare, detection and evaluation are sampled to aluminium oxide.Measuring speed of the present invention is fast, is skillfully constructed, and step is simple, easy to operate, and standard is clear, can judge alumina base in the quality grade of boron content easily and fast.

Description

The method and alumina product grade discrimination of boron are quickly detected in Alpha-alumina
Technical field
The invention belongs to chemical industry measurement field, it is related to detecting the method for boron in aluminium oxide and the grade of alumina product is sentenced Not, specially a kind of method reacted with polyvinyl alcohol by Alpha-alumina to detect the boron content in aluminium oxide, and come with this Judge the grade of alumina product.
Background technology
Alpha-alumina has higher chemical stability, with fusing point is high, thermal stability is good, hardness is big, wearability is good, machine The features such as tool intensity is high, electrical insulating property is good, corrosion-resistant is widely used in sizing, amorphous refractory, castable refractory combination The product scopes such as agent, Wear-resistant Sharper, high-purity refractory fibre, special cermacis, electronic ceramics.The production technology of Alpha-alumina is:Hydrogen After the calcining of additive phase inversion is added in aluminium oxide or aluminium oxide, using advanced grinding technology and technique powder.Al(OH)3 407.30 DEG C are dehydrated and generate γ-Al2O3, γ-Al2O3Start to be changed into θ-Al after 900 DEG C2O3, just turn until 1200 DEG C Turn to α-Al2O3, form stable crystal form.
It is consumed to reduce, shortens the time, reduce cost, it in process of production, generally can outer doping.Additive kind There are many class, wherein commonly one is boric acid, boric acid(H3BO3)For white powder crystallization or three clinopinacoid flakey gloss knots Crystalline substance has satiny feel, and odorless, aqueous solution is weakly acidic, 169 DEG C of fusing point, 300 DEG C of boiling point, is heated to losing at 100 ~ 105 DEG C 1 molecular water and form metaboric acid(HBO2), long-time heating can be changed into pyroboric acid when 104 ~ 160 DEG C(H2B4O7), continue to add Heat then forms anhydride to higher temperature(B2O3), can volatilize with vapor, take away the sodium in product, be conducive to the formation of α phases. Meanwhile it as the reduction of temperature, boric acid and its saline crystallization are precipitated, being attached in calciner, foring boron in calcination atmosphere The atmosphere of acid and its esters, to make α-Al2O3Product processing when, no matter whether additive has boric acid, product that will all possess Certain boron content.In some specific users, the structure and content of boron and its compound, directly determining can produce α-the Al are used in flow2O3Product.Currently without the determination method of structure and content influence for boron and its compound, only Can use in pilot production, be judged according to using effect, in time in cost all generate greatly waste.
Invention content
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, provide one kind by Alpha-alumina and poly- second Enol reaction carrys out the method for quickly detecting the boron content in aluminium oxide, and the grade of alumina product is judged with this.
In order to solve the above technical problems, technical solution proposed by the present invention is:
A kind of method that boron is detected in Alpha-alumina, includes the following steps:
(1)Sampling:Even-grained sample 1000g or so is chosen in production scene, mixing homogenizing passes through three with quartering Secondary division is in weight 125g or so;
(2)Dispensing:In the environment of 25 DEG C of temperature, humidity 60%, in 100ml beakers A, 20.00ml temperature 60 Cs, dense are added The poly-vinyl alcohol solution of degree 10%, adds 10.00g samples;
(3)Gelling:120s is quickly stirred with the glass bar of diameter 5mm, long 200mm, and constant temperature is 60 DEG C, is then allowed to stand 300s, Natural cooling;
(4)Dumping tower tray:Beaker is tilted into 30 ° of inclination angle, beaker mouth face lower section is accepted with the 100ml beakers B of known weight W and burnt α-the Al that cup A is flowed down2O3With the mixture of polyvinyl alcohol, 300 seconds time is accepted;
(5)It weighs:The total weight G of beaker B and mixture are weighed on balance;
(6)It calculates:Mixture flow vector(g)L=G-W calculates α-Al with this mixture flow vector2O3Boron in raw material contains Amount.
A kind of Grade Judgment of the alumina product based on boron content is based on above-mentioned detection method, if final be lost in L >=25g is measured, then the product is top grade product;L >=20g, then the product is certified products;L < 20g, then the product is defective work.
In the present invention, the aluminium hydroxide and aluminium oxide of industrial goods, under normal circumstances, containing 0.1-0.6% sodium oxide molybdenas, Under 1000 DEG C of temperatures above of high temperature, boron forms borax, about 880 DEG C of the fusing point of borax, 1575 DEG C of boiling point with sodium.Finally with borax shape Formula is present in product α-Al2O3Among.At a certain temperature, polyvinyl alcohol reacts to form double diol type gels with borax, is similar to Jelly.Boron content is higher, and the mobility of gel is poorer.Therefore, pass through the mobility of detection gel, you can be accurately judged to raw material In boron content.But in production scene, due to the needs of production process, can not devote a tremendous amount of time repeatedly sampling, Accurate sample preparation is slowly reacted, and needs quickly to detect, rapid results, so the present invention thick sampling appropriate is originally, it is appropriate to add Fast response reacts, and minute is reduced, to achieve the purpose that quickly to detect.
Compared with prior art, the present invention has following advantages:
Detection speed is fast:It can be completed, and make grade discrimination within 15 minutes, particularly suitable for analysis of production control;
It is skillfully constructed:There is no the contents that boron is tested by traditional chemical analysis or physical analysis by the present invention, but lead to The physicochemical characteristic of the occurrence status borax of boron is crossed to detect, is skillfully constructed;
It is easy to operate:Simple for process, easy to operate, general laboratory can effectively implement;
Standard is clear:By mass data acquisition, control, differentiate that precisely top grade product, certified products and defective work are very clear, It can accurately judge the aluminium oxide quality simply by comparison threshold value number.
Specific implementation mode
Below in conjunction with specific preferred embodiment, the invention will be further described, but not thereby limiting the invention Protection domain.
A kind of method that boron is detected in Alpha-alumina, includes the following steps:
(1)Sampling:Even-grained sample 1000g or so is chosen in production scene, mixing homogenizing passes through three with quartering Secondary division is in weight 125g or so;
(2)Dispensing:In the environment of 25 DEG C of temperature, humidity 60%, in 100ml beakers A, 20.00ml temperature 60 Cs, dense are added The poly-vinyl alcohol solution of degree 10%, adds 10.00g samples;
(3)Gelling:120s is quickly stirred with the glass bar of diameter 5mm, long 200mm, and constant temperature is 60 DEG C, is then allowed to stand 300s, Natural cooling;
(4)Dumping tower tray:Beaker is tilted into 30 ° of inclination angle, beaker mouth face lower section is accepted with the 100ml beakers B of known weight W and burnt α-the Al that cup A is flowed down2O3With the mixture of polyvinyl alcohol, 300 seconds time is accepted;
(5)It weighs:The total weight G of beaker B and mixture are weighed on balance;
(6)It calculates:Mixture flow vector(g)L=G-W calculates α-Al with this mixture flow vector2O3Boron in raw material contains Amount.
A kind of Grade Judgment of the alumina product based on boron content is based on above-mentioned detection method, if final be lost in L >=25g is measured, then the product is top grade product;L >=20g, then the product is certified products;L < 20g, then the product is defective work.
The present embodiment is not to be made any form of restriction to shape, material, the structure etc. of the present invention, every according to this hair Bright technical spirit belongs to the technology of the present invention side to any simple modification, equivalent change and modification made by above example The protection domain of case.

Claims (2)

1. the method for quickly detecting boron in Alpha-alumina, which is characterized in that include the following steps:
Sampling:Even-grained sample 1000g or so, mixing homogenizing, with quartering by three times are chosen in production scene Division is in weight 125g or so;
Dispensing:In the environment of 25 DEG C of temperature, humidity 60%, in 100ml beakers A, 25 DEG C of 20.00ml temperature, concentration is added 10% poly-vinyl alcohol solution adds 10.00g samples;
Gelling:120s is quickly stirred with the glass bar of diameter 5mm, long 200mm, and constant temperature is 60 DEG C, is then allowed to stand 300s, it is natural It is cooling;
Dumping tower tray:Beaker is tilted into 30 ° of inclination angle, beaker A is accepted in beaker mouth face lower section with the 100ml beakers B of known weight W α-the Al flowed down2O3With the mixture of polyvinyl alcohol, 300 seconds time is accepted;
It weighs:The total weight G of beaker B and mixture are weighed on balance;
It calculates:Mixture flow vector(g)L=G-W calculates α-Al with this mixture flow vector2O3Boron content in raw material.
2. a kind of Grade Judgment of alumina product based on boron content, which is characterized in that it is based on above-mentioned detection method, if Final number of dropouts L >=25g, then the product is top grade product;L >=20g, then the product is certified products;L < 20g, then the product is not Certified products.
CN201810157667.0A 2018-02-24 2018-02-24 Method for rapidly detecting boron in alpha-alumina and alumina product grade discrimination Active CN108489849B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01250049A (en) * 1988-03-30 1989-10-05 Sando Iron Works Co Ltd Method of measuring concentration of polyvinyl alcohol in aqueous solution
RU2094117C1 (en) * 1996-07-23 1997-10-27 Акционерное общество закрытого типа "Фосфосорб" Sorbent and method for its production
CN2856991Y (en) * 2005-09-09 2007-01-10 卢新 Fast detecting test paper for borax and boric acid in foodstuff
JP2011209306A (en) * 2010-08-02 2011-10-20 Sumitomo Chemical Co Ltd Method for quantitating free boric acid
CN106932385A (en) * 2015-12-30 2017-07-07 中核北方核燃料元件有限公司 The assay method of total Boron contents in boron carbide-aluminum oxide pellet

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01250049A (en) * 1988-03-30 1989-10-05 Sando Iron Works Co Ltd Method of measuring concentration of polyvinyl alcohol in aqueous solution
RU2094117C1 (en) * 1996-07-23 1997-10-27 Акционерное общество закрытого типа "Фосфосорб" Sorbent and method for its production
CN2856991Y (en) * 2005-09-09 2007-01-10 卢新 Fast detecting test paper for borax and boric acid in foodstuff
JP2011209306A (en) * 2010-08-02 2011-10-20 Sumitomo Chemical Co Ltd Method for quantitating free boric acid
CN106932385A (en) * 2015-12-30 2017-07-07 中核北方核燃料元件有限公司 The assay method of total Boron contents in boron carbide-aluminum oxide pellet

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
CAO YUXIA ET AL.: "《Effects of Boron Carbide Content on the Microstructure and Properties of Atmospheric Plasma-Sprayed NiCoCrAlY/Al2O3-B4C Composite Coatings》", 《HERMAL SPRAY TECHNOLOGY》 *
黄栋生 等.: "《Al2O3-B4C弥散芯块烧结过程中硼含量的控制》", 《中南矿冶学院学报》 *

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