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CN104280391A - Method and device for detecting leakage of heat conduction oil - Google Patents

Method and device for detecting leakage of heat conduction oil Download PDF

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Publication number
CN104280391A
CN104280391A CN201410534493.7A CN201410534493A CN104280391A CN 104280391 A CN104280391 A CN 104280391A CN 201410534493 A CN201410534493 A CN 201410534493A CN 104280391 A CN104280391 A CN 104280391A
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China
Prior art keywords
conduction oil
sampling jar
storage tank
oil
oil storage
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CN201410534493.7A
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Chinese (zh)
Inventor
沈海峰
刘松
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JIANGXI SUNWAYS LDK SOLAR POLYSILICON CO Ltd
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JIANGXI SUNWAYS LDK SOLAR POLYSILICON CO Ltd
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Priority to CN201410534493.7A priority Critical patent/CN104280391A/en
Publication of CN104280391A publication Critical patent/CN104280391A/en
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Abstract

The invention discloses a method for detecting the leakage of heat conduction oil. The method is applied to a chlorosilane production process and comprises the following steps: providing a heat conduction oil storage tank, in which the heat conduction oil is stored; providing a first sampling bottle which is connected with the heat conduction oil storage tank through a pipeline, a phenolphthalein alkali liquid is stored in the first sampling bottle and used for detecting the leakage of the heat conduction oil; and providing a second sampling bottle which is connected with the heat conduction oil storage tank through a pipeline, wherein high-purity water is stored in the second sampling bottle for detecting the leakage of the heat conduction oil. In addition, the invention also provides a device for detecting the leakage of the heat conduction oil. According to the method for detecting the leakage of the heat conduction oil, the heat conduction oil storage tank is connected with the first sampling bottle and the second sampling bottle; the liquid is stored in the first sampling bottle and the second sampling bottle; and the leakage of the heat conduction oil and other gases can be quickly judged by observing the liquid condition. The method is simple and is capable of intuitively observing; the leakage can be discovered in time; and the occurrence rate of defective condition is reduced.

Description

Conduction oil leakage detection method and pick-up unit thereof
Technical field
The present invention relates to production technology leak detection field, particularly relate to a kind of conduction oil leakage detection method and pick-up unit thereof.
Background technology
Conduction oil (HO): conduction oil is the former name of " heat medium oil " in GB/T 4016-1983 " petroleum products vocabulary of terms ", English name is Heat transfer oil, for the specialized oil product of a class better heat stability of indirect transfer heat.The occasion of carrying out exchange heat is needed for various.
Because conduction oil boiling point is high, thermal efficiency advantages of higher, has been used in production of polysilicon enterprise in recent years, and the chlorosilane of production of polysilicon enterprise is produced, treatment process, from traditional water heat exchange (comprising steam) process modification be conduction oil heat-exchanging process.Its advantage is: strong chemical reaction not easily occurs for oil and chlorosilane, thus avoids existing employing water as heat exchange, thus decreases the harmfulness of the kickback of water and chlorosilane.
When explained hereafter, if there is chlorosilane gas seepage in conduction oil, the chlorosilane system of high pressure can cause heat-conducting oil system serious overcompression, not only etching apparatus and can cause conduction oil damage and deterioration, thus increases production cost.
And there is no the method that is detected judgement at present, whether seepage chlorosilane gas can be detected in conduction oil fast, when normally finding to occur that state of arts is abnormal in processing processing procedure, process units is parking checking, and does not detect in process of production and control.
Therefore, design that a structure is simple, the conduction oil leakage detection method that can carry out detection control in process of production and pick-up unit thereof be the problem that people endeavour to study always.
Summary of the invention
The object of the present invention is to provide a kind of structure simple, detection seepage can be carried out in process of production, thus prevent the conduction oil leak detection apparatus making state of arts not good brought because of seepage and recovery method thereof.
In order to solve the problems of the technologies described above, the invention provides a kind of conduction oil leakage detection method, in chlorosilane production technology, it comprises the following steps
One conduction oil oil storage tank is provided, inside stores conduction oil;
One first sampling jar is provided, is connected with described conduction oil oil storage tank pipeline, in described first sampling jar, stores the alkali lye adding phenolphthalein, for detecting the leakage scenarios of described conduction oil;
One second sampling jar is provided, is connected with described conduction oil oil storage tank pipeline, in described second sampling jar, stores high purity water, for detecting the leakage scenarios of described conduction oil.
Wherein, described first sampling jar and the second sampling jar are all connected with described conduction oil oil storage tank by gas phase pipeline, and described two gas phase pipelines are equipped with operation valve.
Wherein, described in add phenolphthalein alkali lye be the sodium hydroxide solution adding phenolphthalein, and the concentration of described sodium hydroxide solution is 1% ~ 3%.
Wherein, provide one first sampling jar in step, be connected, store the alkali lye adding phenolphthalein in described first sampling jar with described conduction oil oil storage tank pipeline, for detecting in the leakage scenarios of described conduction oil, concrete steps are:
Regulate the operation valve on described first sampling jar gas phase pipeline, control the air inflow of gas;
The color of alkali lye described in observe and decide, if occur, color is thin out, then represent in described conduction oil oil storage tank have chlorosilane gas seepage; Otherwise, if color is constant, then represent in described conduction oil oil storage tank there is no chlorosilane gas seepage.
Wherein, provide one second sampling jar in step, be connected, store high purity water in described second sampling jar with described conduction oil oil storage tank pipeline, for detecting in the leakage scenarios of described conduction oil, concrete steps are:
Regulate the operation valve on described second sampling jar gas phase pipeline, and control the air inflow of gas;
High purity water situation in second sampling jar described in observe and decide, if there is white precipitate at the bottom of the bottle of described second sampling jar, then illustrate in described conduction oil oil storage tank and be leaked with chlorosilane gas, otherwise, then illustrate in described conduction oil oil storage tank there is no chlorosilane gas seepage.
Correspondingly, present invention also offers a kind of conduction oil leak detection apparatus for realizing above-mentioned conduction oil leakage detection method, for in chlorosilane production technology, it comprises conduction oil oil storage tank, conduction oil is stored in described conduction oil oil storage tank, described conduction oil leak detection apparatus also comprises the first sampling jar and the second sampling jar, described first sampling jar and the second sampling jar are connected on described conduction oil oil storage tank respectively by pipeline, store the alkali lye adding phenolphthalein in described first sampling jar, in described second sampling jar, store water.
Wherein, described first sampling jar and the second sampling jar are all connected with described conduction oil oil storage tank by gas phase pipeline, and described two gas phase pipelines are equipped with operation valve.
Wherein, in described first sampling jar, store the sodium hydroxide solution adding phenolphthalein, and the concentration of described sodium hydroxide solution is 1% ~ 3%.
The detection method of conduction oil seepage provided by the invention, the first sampling jar and the second sampling jar is connected by pipeline on conduction oil oil storage tank, and in the first sampling jar and the second sampling jar, store the alkali lye and the high purity water that add phenolphthalein respectively, the mutual leakage scenarios of conduction oil and other gases can be judged fast by the liquid color situation of observing in sampling jar.Method is simple, and can observe intuitively, thus is convenient to Timeliness coverage leakage scenarios, greatly reduces the incidence of producing undesirable condition.
Accompanying drawing explanation
In order to be illustrated more clearly in technical scheme of the present invention, be briefly described to the accompanying drawing used required in embodiment below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the process flow diagram of the detection method of the conduction oil seepage that embodiment of the present invention provides;
Fig. 2 is the schematic diagram of the conduction oil leak detection apparatus that embodiment of the present invention provides;
Fig. 3 is the apparatus sketch that conduction oil leak detection apparatus that embodiment of the present invention provides is applied to chlorosilane production technology.
Embodiment
Below in conjunction with the accompanying drawing in embodiment of the present invention, the technical scheme in embodiment of the present invention is clearly and completely described.
Refer to Fig. 1, present invention also offers a kind of detection method of conduction oil seepage, be applied in chlorosilane production technology, generate the cold hydrogenation production technology of trichlorosilane in the present embodiment for the catalysis of silicon tetrachloride hydrogenation, concrete steps are as follows:
S1: a conduction oil oil storage tank is provided, inside stores conduction oil.In the present embodiment, the carrying out of conveniently subsequent operation, described conduction oil is cold conditions conduction oil.
S2: provide one first sampling jar, is connected with described conduction oil oil storage tank pipeline, stores the alkali lye adding phenolphthalein in described first sampling jar, for detecting the leakage scenarios of described conduction oil.In the present embodiment, described first sampling jar is connected with described conduction oil oil storage tank by gas phase pipeline, and for the ease of controlling, described gas phase pipeline is provided with operation valve.For the ease of detecting leakage scenarios, described first liquid is the alkali lye adding phenolphthalein.Concrete, described first liquid is the sodium hydroxide solution adding phenolphthalein, and the concentration of described sodium hydroxide solution is 1% ~ 3%.
When judging: the alkali lye color adding phenolphthalein in described first sampling jar is as red.When described conduction oil gets back to described conduction oil oil storage tank after above-mentioned cold hydrogenation process, the operation valve on the described first sampling jar gas phase pipeline of now adjustable control, controls the air inflow of gas.Observe and judge the color of the liquid in described first sampling jar.If color appears in described first liquid, thin out or color becomes colorless, then represent in described conduction oil oil storage tank and be leaked with described silicon tetrachloride gas.Otherwise, if described first liquid color is constant, then represent in described conduction oil oil storage tank there is no described silicon tetrachloride gas permeation.Certainly, in other embodiments, described first liquid also can be other solution, as added the potassium hydroxide of phenolphthalein or other add the alkali lye of phenolphthalein.
S3: provide one second sampling jar, is connected with described conduction oil oil storage tank pipeline, stores high purity water in described second sampling jar, for detecting the leakage scenarios of described conduction oil.In the present embodiment, described second sampling jar is connected with described conduction oil oil storage tank by described gas phase pipeline, and for the ease of controlling, described gas phase pipeline is provided with operation valve.For the ease of observing the leakage scenarios of described conduction oil further intuitively, described second liquid is high purity water.
During judgement: regulate the operation valve on described second sampling jar gas phase pipeline, and control the air inflow of gas, thus be convenient to the accuracy of test structure.Now, by whether there is white precipitate bottom the bottle of the second sampling jar described in visual inspection, if there is precipitation to occur, then illustrate in described conduction oil oil storage tank and be leaked with silicon tetrachloride gas, otherwise, if do not precipitate appearance, then represent in described conduction oil oil storage tank there is no silicon tetrachloride gas permeation.
In addition, adopt PH test paper to test the pH-value of described second liquid, also can judge the gas permeation situation in described conduction oil oil storage tank fast.When being acid when adopting the result of PH test paper test, then represent in described conduction oil oil storage tank have described silicon tetrachloride gas permeation.Otherwise, if result is neutral, then represent in described conduction oil oil storage tank there is no silicon tetrachloride gas permeation.
Be understandable that, a technique in just chlorosilane production is only produced in the cold hydrogenation of above-mentioned employing silicon tetrachloride hydrogenation catalysis generation trichlorosilane, the leakage detection method of above-mentioned conduction oil also can be applicable to other chlorosilane production technologies, as the rectification and purification technique of chlorosilane and the reducing process etc. of polysilicon.
In addition, the detection method of above-mentioned conduction oil seepage also can be applicable to other and adopts acidic materials preparation or processing to need the technique of conduction oil heat exchange, as the production technology of sulfuric acid or production process of hydrochloric acid etc.
The detection method of conduction oil seepage provided by the invention, the first sampling jar and the second sampling jar is connected by pipeline on conduction oil oil storage tank, and liquid is stored in the first sampling jar and the second sampling jar, the mutual leakage scenarios of conduction oil and other gases can be judged fast by the situation of observing liquid.Method is simple, and can observe intuitively, thus is convenient to Timeliness coverage leakage scenarios, greatly reduces the incidence of producing undesirable condition.
See also Fig. 2 to Fig. 3, for the conduction oil leak detection apparatus 100 for realizing above-mentioned conduction oil leakage detection method that embodiment of the present invention provides, in producing for chlorosilane, it comprises conduction oil oil storage tank 10, first sampling jar 20 and the second sampling jar 30, conduction oil is stored in described conduction oil oil storage tank 10, described first sampling jar 20 and the second sampling jar 30 are connected on described conduction oil oil storage tank 10 respectively by pipeline, all liquid is stored in described first sampling jar 20 and the second sampling jar 30, in order to judge that described conduction oil is at the leakage scenarios in chlorosilane production technology.
In the present embodiment, generate the cold hydrogenation production technology of trichlorosilane for the catalysis of silicon tetrachloride hydrogenation.This production process equipment comprises superheater 40 that pipeline successively connects, deposits slag ladle 50, mixer 60 and mixer primary heater 70.Described superheater 40 is connected with described conduction oil oil storage tank 10 pipeline, described conduction oil via pipeline by described superheater 40 and described in deposit slag ladle 50 and absorb heat, raise to make the temperature of described conduction oil.Hydrogen (not shown) and silicon tetrachloride mixed gas (not shown) is stored in described mixer 60, described conduction oil passes through described mixer 60 via pipeline, carry out exchange heat with described hydrogen wherein and silicon tetrachloride mixed gas, raise to make the temperature of described hydrogen and silicon tetrachloride mixed gas.Described mixer primary heater 70 respectively pipeline connects described mixer 60 and described conduction oil oil storage tank 10, described conduction oil carries out exchange heat via pipeline further by described mixer primary heater 70, raise further to make the temperature of described hydrogen and described silicon tetrachloride mixed gas, described conduction oil temperature is got back in described conduction oil oil storage tank 10 after reducing, absorb heat through described superheater 40 again, circulate with this.
In order to judge whether described conduction oil exists the mutual leakage scenarios with silicon tetrachloride gas in above-mentioned production process, when getting back in described conduction oil oil storage tank 10 after described conduction oil carries out heat exchange by above-mentioned production technology, the liquid case in the first sampling jar 20 described in observable and the second sampling jar 30.Concrete, the liquid in described first sampling jar 20 is the alkali lye adding phenolphthalein.In the present embodiment, in order to save the security of cost and guarantee operation further, the liquid in described first sampling jar 20 is the sodium hydroxide solution adding phenolphthalein.During original state, the liquid in described first sampling jar 20 is red.When described conduction oil gets back to described conduction oil oil storage tank 10 after the above-mentioned technological process of production, observe the liquid case in described first sampling jar 20, if now described liquid lighter or become transparent, then illustrate in described conduction oil and be leaked with silicon tetrachloride gas, because silicon tetrachloride gas is sour gas, described silicon tetrachloride gas and described liquid carry out neutralization reaction, generate silicon dioxide and salt, thus the pH-value of described liquid is declined, and then described liquid color shoals or bleach.Otherwise, if the liquid color in described first sampling jar 20 is constant, then represent described conduction oil with in be not leaked with silicon tetrachloride gas.Certainly, in other embodiments, the liquid in described first sampling jar 20 also can be other, as added the potassium hydroxide solution of phenolphthalein or other add the alkaline solution of phenolphthalein.
In the present embodiment, conveniently detect further, described first sampling jar 20 is connected with described conduction oil oil storage tank 10 by gas phase pipeline 21, and described gas phase pipeline 21 is provided with operation valve 211, for controlling the air inflow of described conduction oil oil storage tank 10.Certainly, in other embodiments, described first sampling jar 20 is also connected with described conduction oil oil storage tank 10 by general pipeline.
In the present embodiment, in order to detect the leakage scenarios of the silicon tetrachloride gas in described conduction oil oil storage tank 10 further, the liquid in described second sampling jar 30 is water.When there being silicon tetrachloride gas permeation in described conduction oil oil storage tank 10, described silicon tetrachloride gas is water-soluble, generates silicon dioxide and acid.Now, observe the liquid case in described second sampling jar 30, if there is white precipitate, then illustrate in described conduction oil oil storage tank 10 have silicon tetrachloride gas permeation; Otherwise then represent and do not have.
In addition, in order to further judgement, improve the accuracy of judged result, PH test paper also can be adopted to test the pH-value of the liquid in described second sampling jar 30, if PH test paper is shown as acid value, then represent in described conduction oil oil storage tank 10 have silicon tetrachloride gas permeation.Otherwise, if the neutrality of being shown as, then represent the seepage not having silicon tetrachloride gas in described conduction oil oil storage tank 10.
Conveniently detect, described second sampling jar 30 is connected with described conduction oil oil storage tank 10 by gas phase pipeline 31, and for the ease of regulating and controlling, described meteorological pipeline 31 is provided with operation valve 311, for controlling the air inflow of described conduction oil oil storage tank 10.Certainly, in other embodiments, described second sampling jar 30 is also connected with described conduction oil oil storage tank 10 by general pipeline.
Be understandable that, a technique in just chlorosilane production is only produced in the cold hydrogenation of above-mentioned employing silicon tetrachloride hydrogenation catalysis generation trichlorosilane, described conduction oil leak detection apparatus 100 also can be applicable to other chlorosilane production technologies, as the rectification and purification technique of chlorosilane and the reducing process etc. of polysilicon.
In addition, described conduction oil leak detection apparatus 100 also can be applicable to other and adopts acidic materials preparation or processing to need the technique of conduction oil heat exchange, as the production technology of sulfuric acid or production process of hydrochloric acid etc.
Conduction oil leak detection apparatus provided by the invention by arranging the first sampling jar and the second sampling jar on described conduction oil oil storage tank, and store the alkali lye and the water that add phenolphthalein respectively in the first sampling jar and the second sampling jar, can judge whether conduction oil exists the mutual seepage with chlorosilane in chlorosilane production technology by the liquid color situation of observing in sampling jar, simple operation and can intuitive judgment be carried out by naked eyes, thus can detect in process of production, avoid the abnormal of production technology of bringing because there is seepage to carry out.This apparatus structure is simple, easy and simple to handle, and operating process is short, thus decreases the incidence of producing undesirable condition while greatly increasing production efficiency.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.

Claims (8)

1. a detection method for conduction oil seepage, be applied in chlorosilane production technology, it is characterized in that, it comprises the following steps
One conduction oil oil storage tank is provided, inside stores conduction oil;
One first sampling jar is provided, is connected with described conduction oil oil storage tank pipeline, in described first sampling jar, stores the alkali lye adding phenolphthalein, for detecting the leakage scenarios of described conduction oil;
One second sampling jar is provided, is connected with described conduction oil oil storage tank pipeline, in described second sampling jar, stores high purity water, for detecting the leakage scenarios of described conduction oil.
2. the detection method of conduction oil seepage according to claim 1, is characterized in that, described first sampling jar and the second sampling jar are all connected with described conduction oil oil storage tank by gas phase pipeline, and described two gas phase pipelines are equipped with operation valve.
3. the detection method of conduction oil seepage according to claim 2, is characterized in that, described in add phenolphthalein alkali lye be the sodium hydroxide solution adding phenolphthalein, and the concentration of described sodium hydroxide solution is 1% ~ 3%.
4. the detection method of conduction oil seepage according to claim 3, it is characterized in that, one first sampling jar is provided in step, be connected with described conduction oil oil storage tank pipeline, the alkali lye adding phenolphthalein is stored in described first sampling jar, for detecting in the leakage scenarios of described conduction oil, concrete steps are:
Regulate the operation valve on described first sampling jar gas phase pipeline, control the air inflow of gas;
The color of alkali lye described in observe and decide, if occur, color is thin out, then represent in described conduction oil oil storage tank have chlorosilane gas seepage; Otherwise, if color is constant, then represent in described conduction oil oil storage tank there is no chlorosilane gas seepage.
5. the detection method of conduction oil seepage according to claim 2, is characterized in that, provides one second sampling jar in step, be connected with described conduction oil oil storage tank pipeline, store high purity water in described second sampling jar, for detecting in the leakage scenarios of described conduction oil, concrete steps are:
Regulate the operation valve on described second sampling jar gas phase pipeline, and control the air inflow of gas;
High purity water situation in second sampling jar described in observe and decide, if there is white precipitate at the bottom of the bottle of described second sampling jar, then illustrate in described conduction oil oil storage tank and be leaked with chlorosilane gas, otherwise, then illustrate in described conduction oil oil storage tank there is no chlorosilane gas seepage.
6. one kind for realizing the conduction oil leak detection apparatus of the conduction oil leakage detection method of Claims 1 to 5, for in chlorosilane production technology, it comprises conduction oil oil storage tank, conduction oil is stored in described conduction oil oil storage tank, it is characterized in that, described conduction oil leak detection apparatus also comprises the first sampling jar and the second sampling jar, described first sampling jar and the second sampling jar are connected on described conduction oil oil storage tank respectively by pipeline, store the alkali lye adding phenolphthalein in described first sampling jar, in described second sampling jar, store water.
7. conduction oil leak detection apparatus according to claim 6, is characterized in that, described first sampling jar and the second sampling jar are all connected with described conduction oil oil storage tank by gas phase pipeline, and described two gas phase pipelines are equipped with operation valve.
8. conduction oil leak detection apparatus according to claim 6, is characterized in that, stores the sodium hydroxide solution adding phenolphthalein in described first sampling jar, and the concentration of described sodium hydroxide solution is 1% ~ 3%.
CN201410534493.7A 2014-10-11 2014-10-11 Method and device for detecting leakage of heat conduction oil Pending CN104280391A (en)

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Cited By (1)

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CN112164556A (en) * 2020-11-11 2021-01-01 福州清河源环保科技有限公司 Transformer oil tank with anti-seepage warning function

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CN112164556A (en) * 2020-11-11 2021-01-01 福州清河源环保科技有限公司 Transformer oil tank with anti-seepage warning function
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