CN103028581A - Handling method of sand core crucible used for detecting insoluble quinoline - Google Patents
Handling method of sand core crucible used for detecting insoluble quinoline Download PDFInfo
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- CN103028581A CN103028581A CN2011102945539A CN201110294553A CN103028581A CN 103028581 A CN103028581 A CN 103028581A CN 2011102945539 A CN2011102945539 A CN 2011102945539A CN 201110294553 A CN201110294553 A CN 201110294553A CN 103028581 A CN103028581 A CN 103028581A
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Abstract
The invention discloses a handling method of a sand core crucible used for detecting insoluble quinoline insoluble. The handling method of the sand core crucible used for detecting the insoluble quinoline insoluble includes the following steps: (1) a high temperature burning step: the sand core crucible is placed in a high temperature furnace. The temperature of the high temperature furnace rises to 500 DEG C, the sand core crucible is ensured to be burned for 1.8-2.2 hours under the furnace constant temperature of 500 DEG C, then the high temperature furnace is closed and the door of the high temperature furnace is opened until the temperature of the internal furnace falls to the normal temperature, and then the sand core crucible is taken out and cools to the room temperature; (2) a steam blowing step: the sand core crucible after being burned through the high temperature is blown under a steam generator for 3-5 minutes; (3) a ultrasonic wave cleaning step: the sand core crucible after being blown through steam is moved to an ultrasonic wave cleaner to be cleaned for 8-12 minutes; (4) a drying step: first, the sand core crucible is taken out from the ultrasonic wave cleaner and is washed through distilled water, and then is moved inside a constant temperature drying box with 120+-1 DEG C to be dried for 0.8-1.2 hours. The handling method of the sand core crucible used for detecting the insoluble quinoline is capable of ensuring that the sand core crucible after being used can be handled conveniently, fast and completely in an environment-friendly mode.
Description
Technical field
The present invention relates to the processing method after a kind of chemical analysis equipment uses, be specifically related to a kind of processing method of the core crucible for detection of quinoline insolubles.
Background technology
The method that the quinoline insolubles employing in the oils sample is detected in the laboratory is the core filtration method.The core crucible is to detect to analyze the quantitative analysis utensil that quinoline insolubles is used.
Core crucible system selects porous ceramics raw material and glass to form through high temperature sintering.The core sheet has many fine holes, is the shank of performance filtration, and the filtration by the sand filtration chip obtains required analysis result.
Detect under normal circumstances all transducer set filter cores more of more than ten batches of sample, if but the analytical sample of running into is very special needle-like oils sample, it is just blocked and can't continue to use almost to analyze the filter opening that uses a core sheet in practical operation.This is because behind the quinoline insolubles of core crucible in having analyzed heavy oils sample, can pile up one deck organic impurities and inorganic impurity on the surface of bottom core sheet, organic impurities is the γ resin that is insoluble to quinoline, inorganic impurity mostly is greatly black carbon powder or other impurity, these impurity are that a kind of very tiny particle packing is on the core sheet, if do not do effective removing, the core crucible just can not reuse.General stopping state has two kinds, and a kind of is that mechanical admixture stops up, and another kind is the product Crystallization Plugging.And that often run at present is the former.In order to prevent the Particle Blocking filter opening, usually carry out the processing method of three routines, namely before filtration, sample is carried out pre-filtering, if what use such as ortho-test is the core sheet of 1u, the filter element slice that can add 10u before filtration carries out pre-filtering.Yet, because the sample that the laboratory is analyzed is the sample that contains micro-quinoline insolubles, be that viscous oil class impurity and particle are minimum mostly, carrying out pre-filtering does not have positive effect, and has greatly increased analytical error.
Owing to the detection frequency of laboratory quinoline insolubles is quite high, often can detect more than ten quinoline insolubles in one day, namely discarded after using such as the core after will using, will greatly increase analysis cost.Therefore, the processing method of demanding urgently seeking a kind of core recycling improves analysis efficiency to reduce analysis cost.
Summary of the invention
The objective of the invention is in order to overcome the deficiencies in the prior art, a kind of processing method of the core crucible for detection of quinoline insolubles is provided, it can be convenient, fast, thoroughly, the core crucible after using is processed on environmental protection ground, core crucible after the use and new core crucible can reach same detection effect, and the core crucible can be recycled.
A kind of technical scheme that realizes above-mentioned purpose is: a kind of processing method of the core crucible for detection of quinoline insolubles may further comprise the steps:
The high temperature sintering step, first described core crucible is placed high temperature furnace, the temperature of high temperature furnace is risen to 500 ℃, make the aerobic constant temperature calcination 1.8～2.2 hours under 500 ℃ furnace temperature of described core crucible, close again high temperature furnace and open fire door, make fire box temperature slowly be down to normal temperature, then take out the core crucible and be cooled to room temperature;
The steam blowing step will purge 3～5 minutes through the core crucible behind the high temperature sintering under steam generator;
The Ultrasonic Cleaning step will be cleaned 8～12 minutes in the immigration of the core crucible behind the steam blowing supersonic wave cleaning machine;
Drying steps takes out first the core crucible from supersonic wave cleaning machine, clean with distilled water flushing, moves into 120 ± 1 ℃ thermostatic drying chamber inner drying 0.8～1.2 hour again.
The processing method of above-mentioned core crucible for detection of quinoline insolubles, wherein, when carrying out described high temperature sintering step, described high-temperature furnace door leaves the slit of 8～12mm, makes in the described high temperature furnace high temperature sintering under aerobic state.
The processing method of above-mentioned core crucible for detection of quinoline insolubles wherein, when carrying out described steam blowing step, adopts wood clamp or bamboo tweezer to clamp described core crucible and carries out.
The processing method of above-mentioned core crucible for detection of quinoline insolubles, wherein, when carrying out described Ultrasonic Cleaning step, described supersonic wave cleaning machine uses pure water as cleaning fluid, and hyperacoustic vibration frequency is greater than 20,000 hertz.
The technical scheme of the processing method of the core crucible for detection of quinoline insolubles of the present invention, the cleaning method that mainly adopts high temperature sintering and ultrasonic wave to combine can access used core crucible and processes timely and can reuse; Whole processing procedure need not personnel's nurse, and easy and simple to handle; When cleaning, need not to use chemical reagent, can process to environmental protection the core crucible after using, the core crucible after the use and new core crucible can reach same detection effect, and the core crucible can be recycled.
The specific embodiment
Below by specific embodiment technical scheme of the present invention is elaborated:
The processing method of a kind of core crucible for detection of quinoline insolubles of the present invention may further comprise the steps:
The high temperature sintering step, first the core crucible is placed high temperature furnace, the temperature of high temperature furnace is risen to 500 ℃, make the aerobic constant temperature calcination 1.8～2.2 hours under 500 ℃ furnace temperature of core crucible, close again high temperature furnace and open fire door, make fire box temperature slowly be down to normal temperature, then take out the core crucible and be cooled to room temperature; During calcination fire door is left the slit of 10mm, make in the high temperature furnace high temperature sintering under aerobic state, make organic impurities and inorganic impurity on the core sheet of staying the core crucible bottom change into carbon dioxide, i.e. C-H-O+O
2→ CO
2↑
C+O
2→CO
2↑
The steam blowing step, because core crucible anti-falls, anti-insufficient strength of beaing, in order to remove the impurity such as incinerated organic matter of core sheet surface, adopt wood clamp or bamboo tweezer to clamp through the core crucible behind the high temperature sintering and under steam generator, purge 3～5 minutes;
The Ultrasonic Cleaning step will be cleaned 8～12 minutes in the supersonic wave cleaning machine of the immigration of the core crucible behind steam blowing use pure water as cleaning fluid; Because hyperacoustic vibration frequency is more than 20,000 hertz, the micro-wave that produces is referred to as " cavitation phenomenon " physically, constantly produce rapidly the surface of as " small brushes ", washing away the core sheet with the shock wave of the little cavity formation of vanishing, so within a short period of time just can be clean with the surface clean of core sheet; The effect of Ultrasonic Cleaning is effectively broken away under hyperacoustic effect at the inorganic particle class impurity that the core sheet generates after making high temperature sintering;
Drying steps takes out first the core crucible from supersonic wave cleaning machine, clean with distilled water flushing, moves into 120 ± 1 ℃ thermostatic drying chamber inner drying 0.8～1.2 hour again, namely can reuse.
The high temperature sintering step is a committed step in the processing method of the present invention.After the core crucible uses, the quinoline insolubles of filtering is in the core sheet surface accumulation of core crucible bottom in the oils sample, because quinoline insolubles is organic compound, aerobic calcination meeting is decomposed in high temperature furnace, generates the gases such as the fine particle of some inorganic matters and carbon dioxide.Because being the adhesive of quartz sand and anti-uniform temperature, makes the core sheet, its filter bores has strict restriction to the granularity by material, key is that temperature can not be too high when calcination, because the principle of expanding with heat and contract with cold, excess Temperature can destroy the filter opening of core sheet, even the core sheet is damaged, and excessively low such as calcination temperature, the particulate of the filter opening that stops up the core sheet can't be ashed, not have the effect of the filter opening of dredging core sheet.Therefore, strictly control calcination temperature.Character according to quinoline insolubles, the material that stops up the filter opening of core sheet generally is organic resin or some coal dusts, and these materials can be ashed under certain high temperature, will separate with the filter opening of core sheet after the ashing, so again through the subsequently processing of steam blowing and Ultrasonic Cleaning two steps, the core crucible can processedly totally also can utilize fully again.
The below compares the effect that adopts the new core crucible of one group of core crucible after the disposal methods of the present invention and a group to measure the content of quinoline insolubles in the same coal tar, obtains following table:
In the above-mentioned table:
1. whether the precision of checking new and old core crucible to measure quinoline insolubles content in the same coal tar sample with homogeneity test of variance method F has significant difference:
Selected level of significance α=0.05
Look into the F check table of corresponding α value, the free degree is (5,5) corresponding F α=5.05
Because F
0＜F α, the precision of two group analysis data is that 100 (1-α)=95% time are consistent at confidence level, must make new advances, there is not the conspicuousness error in the precision of quinoline insolubles content in the same coal tar sample of old sand core crucible assay;
2. check the degree of accuracy of quinoline insolubles content in two kinds of same coal tar samples of core crucible assay whether significant difference is arranged:
Selected level of significance α=0.05
Look into t check critical value: free degree f=n1+n2-2=6+6-2=10, check in t
0.05,10=1.812
S: be sample standard deviation, the dispersion degree of expression sample parameter,
I: the natural number from 1 to n,
N: number of samples
Because t＜t
0.05,10=1.812, so there is not systematic error in these two kinds of methods.
Conclusion: quinoline insolubles content does not have a significant difference in two kinds of same coal tar samples of core crucible assay.Newly, old sand core crucible can reach same analytical effect.
Those of ordinary skill in the art will be appreciated that, above embodiment illustrates the present invention, and be not to be used as limitation of the invention, as long as in connotation scope of the present invention, all will drop in claims scope of the present invention variation, the modification of the above embodiment.
Claims (4)
1. the processing method for detection of the core crucible of quinoline insolubles is characterized in that, the treating method comprises following steps:
The high temperature sintering step, first described core crucible is placed high temperature furnace, the temperature of high temperature furnace is risen to 500 ℃, make the aerobic constant temperature calcination 1.8～2.2 hours under 500 ℃ furnace temperature of described core crucible, close again high temperature furnace and open fire door, make fire box temperature slowly be down to normal temperature, then take out the core crucible and be cooled to room temperature;
The steam blowing step will purge 3～5 minutes through the core crucible behind the high temperature sintering under steam generator;
The Ultrasonic Cleaning step will be cleaned 8～12 minutes in the immigration of the core crucible behind the steam blowing supersonic wave cleaning machine;
Drying steps takes out first the core crucible from supersonic wave cleaning machine, clean with distilled water flushing, moves into 120 ± 1 ℃ thermostatic drying chamber inner drying 0.8～1.2 hour again.
2. the processing method of the core crucible for detection of quinoline insolubles according to claim 1, it is characterized in that, when carrying out described high temperature sintering step, described high-temperature furnace door leaves the slit of 8～12mm, makes in the described high temperature furnace high temperature sintering under aerobic state.
3. the processing method of the core crucible for detection of quinoline insolubles according to claim 1 is characterized in that, when carrying out described steam blowing step, adopts wood clamp or bamboo tweezer to clamp described core crucible and carries out.
4. the processing method of the core crucible for detection of quinoline insolubles according to claim 1, it is characterized in that, when carrying out described Ultrasonic Cleaning step, described supersonic wave cleaning machine uses pure water as cleaning fluid, and hyperacoustic vibration frequency is greater than 20,000 hertz.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109500015A (en) * | 2018-11-02 | 2019-03-22 | 云南省粮油科学研究院（云南省粮油产品质量监督检验测试中心） | A kind of cleaning method not measuring small-bore glassware internal grease |
| CN110386601A (en) * | 2019-06-24 | 2019-10-29 | 鞍钢股份有限公司 | A method of removal carbon microspheres surface quinoline non-soluble composition granule |
| CN111482423A (en) * | 2020-04-08 | 2020-08-04 | 四川富乐德科技发展有限公司 | Cleaning regeneration method of titanium crucible |
| CN112834382A (en) * | 2021-04-06 | 2021-05-25 | 枣庄杰富意振兴化工有限公司 | Method for detecting content of quinoline insoluble substances |
| CN114682589A (en) * | 2022-04-11 | 2022-07-01 | 云南磷化集团有限公司 | Method for washing quinoline phosphomolybdate precipitate remained in glass sand core crucible |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109500015A (en) * | 2018-11-02 | 2019-03-22 | 云南省粮油科学研究院（云南省粮油产品质量监督检验测试中心） | A kind of cleaning method not measuring small-bore glassware internal grease |
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| CN111482423A (en) * | 2020-04-08 | 2020-08-04 | 四川富乐德科技发展有限公司 | Cleaning regeneration method of titanium crucible |
| CN112834382A (en) * | 2021-04-06 | 2021-05-25 | 枣庄杰富意振兴化工有限公司 | Method for detecting content of quinoline insoluble substances |
| CN114682589A (en) * | 2022-04-11 | 2022-07-01 | 云南磷化集团有限公司 | Method for washing quinoline phosphomolybdate precipitate remained in glass sand core crucible |
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| CN103028581B (en) | 2014-10-22 |
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Effective date of registration: 20170531 Address after: 016011 thousand mile Mountain Industrial Park, Haibowan District, the Inner Mongolia Autonomous Region, Wuhai Patentee after: WUHAI BAOHUA WANCHEN COAL CHEMICAL CO.,LTD. Address before: 200942 Baoshan District Shanghai Baoshan Iron and steel plant in the area of chemical office building road, three Patentee before: Shanghai Baosteel Chemical Co.,Ltd. |
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Address after: 016000 QIANLISHAN Industrial Park, Haibowan District, Wuhai City, Inner Mongolia Autonomous Region Patentee after: Wuhai Baoqi Carbon Materials Co.,Ltd. Address before: 016011 QIANLISHAN Industrial Park, Haibowan District, Wuhai City, Inner Mongolia Autonomous Region Patentee before: WUHAI BAOHUA WANCHEN COAL CHEMICAL CO.,LTD. |