CN108106960A - A kind of method of quick measure chemical durability of glass - Google Patents

A kind of method of quick measure chemical durability of glass Download PDF

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Publication number
CN108106960A
CN108106960A CN201611050270.9A CN201611050270A CN108106960A CN 108106960 A CN108106960 A CN 108106960A CN 201611050270 A CN201611050270 A CN 201611050270A CN 108106960 A CN108106960 A CN 108106960A
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glass
msub
reaction vessel
water
quality
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程谟杰
王秀玲
区定容
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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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

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Analytical Chemistry (AREA)
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Abstract

The invention discloses a kind of method of quick measure chemical durability of glass, this method is the stability test especially suitable for high temperature seal glass based on the test to stability, glass.Specifically include following steps:(1) glass to be measured is crushed and sieved;(2) it is m to weigh quality0Glass particle mixed with water, be placed in reaction vessel, add additive;(3) reaction vessel is closed, reacts more than 5min in 180~240 DEG C;(4) product separates, and solid powder is cleaned, weighs quality after drying, is denoted as m1;(5) the extent of corrosion C of glass is calculated according to the following formula:

Description

A kind of method of quick measure chemical durability of glass
Technical field
The invention belongs to physicochemical property testing fields, and in particular to a kind of method of quick measure chemical durability of glass, Measure especially suitable for high temperature seal glass chemical stability.
Background technology
Glassware can be subject to surrounding medium (such as big gas and water, acid, alkali, salt and other chemical substances in use Deng) corrode, glass resists the ability of this erosion as the chemical stability of glass.Chemical stability is one of glass important One of property and the important indicator of measurement glassware quality good or not.For high temperature seal glass, during sealing-in Hot environment will increase the erosive velocity of glass, reduce its stability, glass sealing will be caused to fail when serious.At present in glass In glass industry, testing the method for chemical durability of glass mainly has surface method (also known as bulk SAMPLE METHOD) and powder method.
Surface method is to represent journey that glass weathers with the generated alkali in the unit interval on unit area or weight loss Degree.This method can not only reflect the characteristic of glass surface, and can reflect the characteristic of glass material itself.But this method needs The surface area of sample is accurately measured, thus it is more demanding for the shape and size of glass specimen, while to glass surface matter Amount requirement is also high.For the not high glass of in irregular shape or surface quality, its surface area can not be accurately calculated, and due to Test sample volume is larger, and the testing time is long, thus its application range is very limited.
Powder method, its essence is the glass specimen that will have certain granules degree, in certain solution (water, acid or alkali etc.) into Row corrodes, and finally measures the weight or generated alkali of dust losses.This method is simple, effectively, and shape to glass specimen and Surface quality does not require, therefore can measure the chemical stability of various glasswares.But this method is by granular size and The influence of the factors such as the ratio between evenness, glass thermal history, staining fluid and sample weight.And due to the relatively high stabilization of glass Property so that traditional powder measuring method take it is longer, generally require several days even the several months.
To overcome the shortcomings of existing assay method, improve measure efficiency and accuracy rate, it is necessary to seek new assay method. The present invention provides a kind of assay method of simple and practicable, accurate quickly chemical durability of glass, steady to improve the chemistry of glass It is qualitative to provide foundation.
The content of the invention
It is an object of the present invention to for existing test method to glass specimen geomery, granularity requirement height, test The problems such as time is long, the present invention provide a kind of method of quick measure chemical durability of glass, and this method is simple and practicable, and test Process is influenced smaller by extraneous factor, and measurement is accurate.
Technical scheme is as follows:
A kind of method of quick measure chemical durability of glass, is as follows:
(1) glass to be measured is crushed and sieved;
(2) it is m to weigh quality0Glass particle mixed with water, be placed in reaction vessel, add additive, additive with The mass ratio of water is 1:50~1:Between 200;
(3) reaction vessel is closed, reacts more than 5min in 180~240 DEG C;
(4) product carries out separation of solid and liquid, and solid powder is cleaned, weighs quality after drying, is denoted as m1
(5) extent of corrosion C of the glass in additive aqueous solution is calculated according to the following formula:
Glass smashes it through 20~60 mesh sieves in step (1), takes the component by sieve.
The mass ratio of glass and water is 1 in step (2):20~1:Between 50, the volume of water for reactor volume 20~ Between 60%.
The container equipped with reactant is placed in temperature in step (3) is in 180~240 DEG C of baking oven, pressure for 1002~ 3345kPa, preferably pressure are 1.55 ± 0.15MPa, and constant temperature handles 5~30min with this condition, take out reaction vessel and are cooled to Room temperature.
Additive therefor is any one in the acetic acid of the hydrochloric acid of 2M, the sulfuric acid of 1M, the nitric acid of 2M, the phosphoric acid of 1M, 2M.
The optimal conditions of reaction are 200 ± 5 DEG C, and the reaction time is 15 ± 1min.
The precision of mass measurement reaches 0.0001g.
Glass to be measured is silicate, any one in borate, phosphate glass.
Advantage of the invention is that:
(1) a kind of simple, quick method for measuring chemical durability of glass is provided, will originally need several days or even several months Test taper in even shorter time a few houres and complete, greatly improve the efficiency of test.
(2) test carries out in completely closed reactor, and experiment process is influenced smaller, measurement standard by extraneous factor Really.
(3) test method to glass sample shape, size and granularity without too big requirement, therefore can be extensive For the measure of various glass.
Specific embodiment
The present invention is further described below by specific embodiment
Embodiment 1:
(1) glass is high temperature seal glass used by, and raw material composition is listed in Table 1 below, and 40 mesh sieves are crossed after glass breaking;
(2) weigh the glass particle that quality is 1.0000g to mix with 30mL water, be placed in autoclave, add concentration For the hydrochloric acid 0.5mL of 1M;
(3) autoclave is placed in 200 DEG C of baking oven, and constant temperature processing 15min, it is cold to take out reaction vessel with this condition But to room temperature;
(4) product is separated by filtration, and it is 0.2175g that solid powder is cleaned, quality is weighed after drying;
(5) the extent of corrosion C of glass is calculated according to the following formula:
Embodiment 2:
(1) glass is high temperature seal glass used by, and raw material composition is listed in Table 1 below, and 40 mesh sieves are crossed after glass breaking;
(2) weigh the glass particle that quality is 1.0000g to mix with 50mL water, be placed in autoclave, add concentration For the sulfuric acid solution 1mL of 2M;
(3) autoclave is placed in 200 DEG C of baking oven, and constant temperature processing 15min, it is cold to take out reaction vessel with this condition But to room temperature;
(4) product is separated by filtration, and it is 0.0763g that solid powder is cleaned, quality is weighed after drying;
(5) the extent of corrosion C of glass is calculated according to the following formula:
Embodiment 3:
(1) glass is quartz glass used by, and raw material composition is listed in Table 1 below, and 60 mesh sieves are crossed after glass breaking;
(2) weigh the glass particle that quality is 1.0000g to mix with 30mL water, be placed in autoclave, add concentration For the salpeter solution 0.2mL of 2M;
(3) autoclave is placed in 200 DEG C of baking oven, and constant temperature processing 15min, it is cold to take out reaction vessel with this condition But to room temperature;
(4) product is separated by filtration, and it is 0.6954g that solid powder is cleaned, quality is weighed after drying;
(5) the extent of corrosion C of glass is calculated according to the following formula:
Embodiment 4:
(1) glass is common building glass used by, and raw material composition is listed in Table 1 below, and 40 mesh sieves are crossed after glass breaking;
(2) weigh the glass particle that quality is 1.0000g to mix with 20mL water, be placed in autoclave, add 2M's Acetum 0.4mL;
(3) autoclave is placed in the baking oven of 200 DEG C (pressure 1554kPa), and constant temperature is handled with this condition 15min takes out reaction vessel and is cooled to room temperature;
(4) product is separated by filtration, and it is 0.0183g that solid powder is cleaned, quality is weighed after drying;
(5) the extent of corrosion C of glass is calculated according to the following formula:
In 1 embodiment of table the composition (molar content) of glass used and experiment after extent of corrosion
As seen from table:SiO in glass ingredient2Content it is higher, experiment post-etching degree it is lower, illustrate SiO2Content is high Glass has higher chemical stability.The glass of alkaline including earth metal oxide is than the glass corrosion degree of alkali metal containing oxide Low, illustrating the glass of alkaline including earth metal oxide has higher chemical stability.

Claims (8)

  1. A kind of 1. method of quick measure chemical durability of glass, it is characterised in that be as follows:
    (1) glass to be measured is crushed and sieved;
    (2) it is m to weigh quality0Glass particle mixed with water, be placed in reaction vessel, add additive, the matter of additive and water Ratio is measured 1:50~1:Between 200;
    (3) reaction vessel is closed, reacts more than 5min in 180~240 DEG C;
    (4) product carries out separation of solid and liquid, and solid powder is cleaned, weighs quality after drying, is denoted as m1
    (5) extent of corrosion C of the glass in additive aqueous solution is calculated according to the following formula:
    <mrow> <mi>C</mi> <mo>=</mo> <mfrac> <mrow> <msub> <mi>m</mi> <mn>0</mn> </msub> <mo>-</mo> <msub> <mi>m</mi> <mn>1</mn> </msub> </mrow> <msub> <mi>m</mi> <mn>0</mn> </msub> </mfrac> <mo>&amp;times;</mo> <mn>100</mn> <mi>%</mi> <mo>.</mo> </mrow>
  2. 2. the method as described in claim 1, which is characterized in that glass smashes it through 20~60 mesh sieves in step (1), takes and passes through The component of sieve.
  3. 3. the method as described in claim 1, which is characterized in that the mass ratio of glass and water is 1 in step (2):20~1:50 Between, the volume of water is between the 20~60% of reactor volume.
  4. 4. the method as described in claim 1, which is characterized in that the container equipped with reactant is placed in temperature in step (3) is In 180~240 DEG C of baking oven, pressure is 1002~3345kPa, and preferably pressure is 1.55 ± 0.15MPa, with this condition constant temperature 5~30min is handled, reaction vessel is taken out and is cooled to room temperature.
  5. 5. the method as described in claim 1, which is characterized in that additive therefor is the hydrochloric acid of 2M, the sulfuric acid of 1M, the nitre of 2M Acid, the phosphoric acid of 1M, 2M acetic acid in any one.
  6. 6. method as described in claim 1 or 4, which is characterized in that the optimal conditions of reaction are 200 ± 5 DEG C, and the reaction time is 15±1min。
  7. 7. the method as described in claim 1, which is characterized in that the precision of mass measurement reaches 0.0001g.
  8. 8. the method as described in claim 1, which is characterized in that glass to be measured is silicate, in borate, phosphate glass Any one.
CN201611050270.9A 2016-11-25 2016-11-25 A kind of method of quick measure chemical durability of glass Pending CN108106960A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110579421A (en) * 2019-09-12 2019-12-17 安徽神剑新材料股份有限公司 Powder coating storage stability testing method

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104215567A (en) * 2013-08-27 2014-12-17 芜湖东旭光电装备技术有限公司 Method for testing glass chemical stability
CN104280333A (en) * 2013-08-27 2015-01-14 东旭集团有限公司 Method for measuring chemical stability of glass based on glass column

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104215567A (en) * 2013-08-27 2014-12-17 芜湖东旭光电装备技术有限公司 Method for testing glass chemical stability
CN104280333A (en) * 2013-08-27 2015-01-14 东旭集团有限公司 Method for measuring chemical stability of glass based on glass column

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
"玻璃工艺学"教材选编小组: "《玻璃工艺学》", 30 September 1961, 中国工业出版社 *
国家技术监督局: "无色光学玻璃化学稳定性试验方法", 《GB/T 17129-1997 中华人民共和国国家标准》 *
国家技术监督局: "滤光玻璃测试方法 化学稳定性", 《GB/T 15489.7-1995 中华人民共和国国家标准》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110579421A (en) * 2019-09-12 2019-12-17 安徽神剑新材料股份有限公司 Powder coating storage stability testing method

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