NL2031437B1 - Carbon monoxide gas-sensitive micro-capsules, preparation method, and method for identifying source of ignition in worked-out section - Google Patents
Carbon monoxide gas-sensitive micro-capsules, preparation method, and method for identifying source of ignition in worked-out section Download PDFInfo
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- NL2031437B1 NL2031437B1 NL2031437A NL2031437A NL2031437B1 NL 2031437 B1 NL2031437 B1 NL 2031437B1 NL 2031437 A NL2031437 A NL 2031437A NL 2031437 A NL2031437 A NL 2031437A NL 2031437 B1 NL2031437 B1 NL 2031437B1
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 85
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910002091 carbon monoxide Inorganic materials 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000007789 gas Substances 0.000 claims abstract description 129
- 239000011162 core material Substances 0.000 claims abstract description 55
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims abstract description 18
- 238000010557 suspension polymerization reaction Methods 0.000 claims abstract description 9
- 231100000252 nontoxic Toxicity 0.000 claims abstract description 7
- 230000003000 nontoxic effect Effects 0.000 claims abstract description 7
- 238000001514 detection method Methods 0.000 claims abstract description 5
- 239000011258 core-shell material Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 30
- 239000003245 coal Substances 0.000 claims description 27
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical group C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 26
- 239000007787 solid Substances 0.000 claims description 25
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 23
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 20
- 239000011257 shell material Substances 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical group CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 239000012074 organic phase Substances 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- 239000003431 cross linking reagent Substances 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000003999 initiator Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 2
- 238000003892 spreading Methods 0.000 claims description 2
- 230000007480 spreading Effects 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000008346 aqueous phase Substances 0.000 claims 2
- 238000004090 dissolution Methods 0.000 claims 2
- 238000005119 centrifugation Methods 0.000 claims 1
- 238000007873 sieving Methods 0.000 claims 1
- 238000002485 combustion reaction Methods 0.000 abstract description 25
- 230000002269 spontaneous effect Effects 0.000 abstract description 25
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 26
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 16
- 229940068984 polyvinyl alcohol Drugs 0.000 description 16
- 229940087305 limonene Drugs 0.000 description 13
- 235000001510 limonene Nutrition 0.000 description 13
- 239000012071 phase Substances 0.000 description 11
- 229940044603 styrene Drugs 0.000 description 11
- 229940116441 divinylbenzene Drugs 0.000 description 10
- 210000003739 neck Anatomy 0.000 description 8
- 238000006116 polymerization reaction Methods 0.000 description 8
- 239000002775 capsule Substances 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 208000003629 Rupture Diseases 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000011435 rock Substances 0.000 description 3
- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 description 2
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 description 2
- 239000000306 component Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000001525 mentha piperita l. herb oil Substances 0.000 description 2
- 229940041616 menthol Drugs 0.000 description 2
- 238000005065 mining Methods 0.000 description 2
- 235000019477 peppermint oil Nutrition 0.000 description 2
- 241000132092 Aster Species 0.000 description 1
- 201000004569 Blindness Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000002817 coal dust Substances 0.000 description 1
- 229940000425 combination drug Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229940057952 methanol Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/126—Composition of the body, e.g. the composition of its sensitive layer comprising organic polymers
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/128—Microapparatus
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/004—CO or CO2
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
Disclosed in the present disclosure is carbon monoxide gas— sensitive micro—capsules. Each micro—capsule is of "core—shell" structure, including core and wall shell cladded outside core; The micro—capsules are obtained by suspension polymerization; and wall shell ruptures after contacting CO gas, and core located inside wall shell releases non—toxic and harmless gases. Disclosed in the present disclosure is also a preparation method of carbon monoxide gas—sensitive micro—capsules, and a method for identifying source of ignition in worked—out section by carbon monoxide gas—sensitive micro—capsules. Palladium dichloride is added into wall shells of gas micro—capsules. In carbon monoxide environment, shells of gas— sensitive micro—capsules rupture due to reaction between palladium dichloride and carbon monoxide, releasing gases volatilized from core materials. Whether there is spontaneous combustion of residual coals is determined by detection of gases of core materials.
Description
CARBON MONOXIDE GAS-SENSITIVE MICRO-CAPSULES, PREPARATION METHOD,
AND METHOD FOR IDENTIFYING SOURCE OF IGNITION IN WORKED-OUT
SECTION
The present disclosure belongs to the technical field of the prevention and control of spontaneous combustion disasters of coals in mines, and particularly relates to carbon monoxide gas- sensitive micro-capsules, a preparation method, and a method for identifying a source of ignition in a worked-out section.
Spontaneous combustion of residual coals in worked-out sec- tions can produce toxic and harm gases, which can lead to gas and coal dust explosions as sources of ignition, and even, poses a se- vere threat on the safety mining of coal mines. The spontaneous combustion of coals occurs after a laggard oxidation stage (gener- ally, before 70°C), at which coal temperature elevates slowly. Af- ter the temperature exceeds 70°C, the coals approach a rapid oxida- tion stage, at which the coal temperature will elevate quickly in an exponential form. Therefore, after spontaneous combustion dis- asters of the coals happen, it is necessary to take measures for governance in a timely manner, since it is difficult to control in the rapid oxidation stage. In addition, the worked-out sections are huge spaces where broken coal rocks are filled, and working personnel can't access to. After the spontaneous combustion of the residual coals happens in the worked-out sections, locations at which the spontaneous combustion happens are not easy to determine accurately, which causes the blindness of governance on the spon- taneous combustion of the residual coals in the worked-out sec- tions, and restricts the effectiveness of hazard control. There- fore, it is of great importance to invent the monitoring and early warning of the spontaneous combustion disasters of the residual coals in the worked-out sections and an effective method for quickly determining areas where the spontaneous combustion disas- ters happen.
As the broken coal rocks with low thermal conductivity are filled in the worked-out sections, the long-distance propagation of the temperature, electricity, magnetism, and other signals fails to achieve in the worked-out sections. Spontaneous combus- tion signals of the coals are transferred from the inside to the outside (coal faces) of the worked-out sections mainly by the gas- es as carriers. CO is a representative gas in the spontaneous com- bustion disasters of the coals. At present, whether there are the spontaneous combustion disasters of the coals in the worked-out sections is determined mainly by monitoring whether there is the
CO gas or whether there is any continual elevation in the concen- tration of the CO gas at upper corners of coal faces in the coal mines. However, the CO gas is diluted easily by leaked air and ad- sorbed by the residual coals easily in the worked-out sections.
Generally, the production of the CO gas and changes in its concen- tration can't be monitored accurately, resulting in failure in the timely detection of the spontaneous combustion disasters of the residual coals.
A micro-capsule technology is such that solids, liquids, or gases are wrapped by natural or synthesized high molecular materi- als to form semi-permeable or sealed capsule membranes. Under spe- cific conditions, such as, temperature, pH, and water solubility, shells of micro-capsules are decomposed, so that core materials achieve a deserved effect. At present, although there are many temperature-sensitive micro-capsules that have been developed, fewer and fewer reports on gas-sensitive micro-capsules are found.
At the preliminary stage of the spontaneous combustion of the coals, the sources of ignition have low temperature and small vol- ume, the coal rocks have low thermal conductivity coefficients, and in most cases, the temperature-sensitive micro-capsules close to the sources of ignition can also not sense the temperature of the sources of ignition, resulting in failure to make responses quickly.
However, at the preliminary stage of the spontaneous combus- tion of the coals, a large amount of CO gas will be produced throughout the process of the spontaneous combustion, and thus, the development of the gas-sensitive micro-capsules specific to the CO gas will have an important significance.
In view of the above, the present application puts forward carbon monoxide gas-sensitive micro-capsules. In a carbon monoxide atmosphere, after shells of the micro-capsules rupture under a re- action with carbon monoxide, the micro-capsules will release cores, which will be changed into the gases quickly by evapora- tion; and after the gases are detected by a monitoring analysis meter at the upper corner of the coal face, the spontaneous com- bustion of the residual coals can be determined quickly. In addi- tion, if the carbon monoxide gas-sensitive micro-capsules with different types of cores are sprayed in different areas of the worked-out sections, areas where the spontaneous combustion of the residual coals happens can be determined according to varieties of the detected core gases.
The present disclosure aims to provide a carbon monoxide gas- sensitive micro-capsule, a preparation method, and a method for identifying a source of ignition in a worked-out section in order to overcome the above defects in the prior art.
In order to fulfill the above objective, technical solutions of the present disclosure are as follow:
Each carbon monoxide gas-sensitive micro-capsule shows a "core-shell" structure, which includes a core and a wall shell cladded outside the core;
The wall shell is clad shell consisting of styrene polymer and palladium dichloride; the wall shell material comprises sty- rene, the palladium dichloride, a dispersant, a cross-linking agent, and an initiator; and the core material is a volatile sub- stance that can volatilize non-toxic and harmless gases. The gas- sensitive micro-capsules are obtained by suspension polymeriza- tion;
The wall shell ruptures after contacting CO gas, and the core positioned in the wall shell releases non-toxic and harmless gas- es.
Preferably, the dispersant is polyvinyl alcohol, the cross- linking agent is divinyl benzene, and the initiator is diisopropyl azodicarboxylate.
The present disclosure further discloses a preparation method of a carbon monoxide gas-sensitive micro-capsule.
The preparing method of the carbon monoxide gas-sensitive mi- cro-capsule includes the following steps:
Step 11: weighing a certain mass of polyvinyl alcohol and putting into a first beaker for heating; after the polyvinyl alco- hol is changed from white granular solids into colorless transpar- ent viscous liquid, adding distilled water into the first beaker; and then, transferring the first beaker and a mixture therein in an ultrasonic cleaner and heating for ultrasonic dissolving, so that the polyvinyl alcohol is dispersed in the distilled water completely and uniformly to form a water phase solution;
Step 12: weighing a certain mass of the styrene, the divinyl benzene, the diisopropyl azodicarboxylate, the palladium dichlo- ride, and the core materials, adding them into a second beaker, and stirring a mixture in the second beaker, so that the mixture is mixed fully to form an organic phase solution;
Step 13: pouring the water phase solution in the first beak- er, and the organic phase solution in the second beaker into a flask with three necks, positioned in a constant temperature oil- bath pan, and stirring for the suspension polymerization;
Step 14: after the suspension polymerization ends, pouring an obtained solid-liquid mixture into a third beaker for standing and suction filtration, and obtaining solid particles; and washing the obtained solid particles centrifugally for three times with metha- nol to wash off organic substances left on surfaces of the solid particles, and finally, drying, and obtaining micro-capsules with- out residual moisture;
Step 15: screening the micro-capsules obtained in the step 14, and obtaining the carbon monoxide gas micro-capsules.
Preferably, in the step 11, a mass ratio of the polyvinyl al- cchol to the distilled water is 1:500.
Preferably, in the step 11, the polyvinyl alcohol in the first beaker is heated at a heating temperature of 80°C in a ther- mostat water bath kettle;
Time for which the first beaker and the mixture therein are heated in the ultrasonic cleaner for ultrascnic dissolving is 10 h.
Preferably, in the step 12, a mass ratio of the polyvinyl alcohol to the core material is 0.1-0.14:1; 5 a mass ratio of the styrene to the core material is 1.6- 2.4:1; a mass ratio of the divinyl benzene to the core material is 0.08-0.12:1; a mass ratio of the diisopropyl azodicarboxylate to the core material is 0.4-0.8:1; a mass ratio of the palladium dichloride to the core material is 0.1-0.2:1.
Preferably, in the step 12, the mixture in the second beaker is stirred with a magnetic stirring apparatus for 2 h to 4 h.
Preferably, in the step 13, the temperature of the thermostat water bath kettle is 80°C; stirring the mixture in the flask with three necks for 5 h with a mechanical stirrer, wherein a stirring speed of the mechan- ical stirrer is 300 r/min.
Preferably, in the step 15, a particle size of each screened carbon monoxide gas micro-capsule ranges from 120 pm to 250 pm.
The present disclosure further discloses a method for identi- fying a source of ignition in a worked-out section with the carbon monoxide gas-sensitive micro-capsules.
The method for identifying the source of ignition in the worked-out section with the carbon monoxide gas-sensitive micro- capsules includes the following steps:
Step 21: preparing the carbon monoxide gas-sensitive micro- capsules that can release different gases from different core ma- terials;
Step 22: as a coal face is pushed ahead, dividing areas in the worked-out section at a rear of the coal face, and spreading the carbon monoxide gas-sensitive micro-capsules prepared from different core materials in the divided areas, wherein a width of each area ranges from 10 m to 20 m;
Step 23: arranging a detecting instrument at an upper corner of the coal face, collecting gases in the worked-out section at the upper corner, and detecting gas varieties; and once detecting that the cores containing the carbon monoxide gas-sensitive micro- capsules release gases, giving an alarm immediately;
Step 24: determining an area where spontaneous combustion disasters of coals happen in the worked-out section by a worker according to the varieties of the detected core gases.
The present disclosure has the following beneficial effects:
The carbon monoxide gas-sensitive micro-capsules of the pre- sent disclosure are obtained by the suspension polymerization; the wall shell material includes the styrene, the polyvinyl alcohol, the divinyl benzene, the diisopropyl azodicarboxylate, and the palladium dichloride, where the styrene is used as a monomer of the wall material, the polyvinyl alcohol is used as the disper- sant, the divinyl benzene is used as the cross-linking agent, and the diisopropyl azodicarboxylate is used as the initiator; during polymerization, the wall shell material is polymerized into a ball to clad the core material; and the palladium dichloride in the wall shell can react with the CO gas. In carbon monoxide environ- ment, the wall shells of the gas-sensitive micro-capsules of the present disclosure rupture due to a reaction between the palladium dichloride and the carbon monoxide, releasing the gases volati- lized from the core materials. Whether there is the spontaneous combustion of the residual coals can be determined by the detec- tion of the gases of the core materials.
After the carbon monoxide gas-sensitive micro-capsules with different types of core materials are spread in different areas of the worked-out sections, areas where the spontaneous combustion of the residual coals happens can be determined according to varie- ties of the detected core gases.
The drawings of the specification constituting one part of the present application are described for further understanding the present disclosure. The illustrative embodiments of the pre- sent disclosure and descriptions thereof are illustrative of the present application, and are not construed as an improper limita- tion to the present application.
FIG. 1 is a schematic diagram illustrating carbon monoxide gas-sensitive micro-capsules positioned in a high pressure- resistant porous ball in the present disclosure;
FIG. 2 is an arrangement diagram illustrating spraying of carbon monoxide gas-sensitive micro-capsules in a worked-out sec- tion in the embodiment 4;
It should be noted that the following detailed descriptions are exemplary, which are intended to further explain the present application. Unless otherwise indicated, all technical and scien- tific terms used herein have the same meaning as commonly under- stood by a person of ordinary skill in the art to which the pre- sent application pertains.
It is worthwhile to note that terms used here are not intend- ed to limit the illustrative implementations according to the pre- sent application, but are merely descriptive of the implementa- tions. Unless otherwise directed by the context, singular forms of terms used here are intended to include plural forms. Besides, it will be also appreciated that when terms “contain” and/or “in- clude” are used in the specification, it is indicated that charac- teristics, steps, operations, devices, assemblies, and/or a combi- nation thereof exist.
In the present disclosure, "up", "down", "bottom", "top", and other terms indicating directions or positional relationships rep- resent directions or positional relationships shown in the draw- ings. They are relational words determined merely for describing structural relationships between components or elements of the present disclosure, but are not intended to indicate any one com- ponent or element in the present disclosure, which aren't con- strued as a limitation to the present disclosure.
In the present disclosure, terms "link", "connect", and other terms should be broadly understood. For example, the terms may re- fer to fixed connection and may also refer to integrated connec- tion or detachable connection. The terms may refer to direct con- nection, and may also refer to indirect connection through a medi- um. For a person researched or skilled in the art, specific mean- ings of these terms in the present disclosure can be determined according to the specific condition, which aren't construed as a limitation to the present disclosure.
The present disclosure will be further explained with refer- ence to drawings and embodiments.
Embodiment 1:
Preparation of a water phase: 0.5 g of polyvinyl alcohol is weighed and put into a first beaker, and then, is heated in a thermostat water bath kettle at 80°C, so that it is changed from white granular solids into colorless transparent viscous liquid; and 250 ml of distilled water is added into the first beaker, the first beaker is transferred in an ultrasonic cleaner and heated for ultrasonic dissolving for 10 h, until the polyvinyl alcohol is dispersed in water completely and uniformly to form a water phase solution;
Preparation of an organic phase:8 g of styrene, 0.4 g of divinyl benzene, 2 g of diisopropyl azodicarboxylate, 0.5 g of palladium dichloride, and 5 g of limonene are weighed and put into a second beaker, and then, a mixture is stirred for 3 h with a magnetic stirring apparatus to be mixed fully and uniformly;
A polymerization reaction: a 500 ml flask with three necks is put into a constant temperature oil-bath pan at a temperature of 80°C, the prepared water phase and the organic phase are poured into the 500 ml flask with three necks with stirring, and then, a polymerization reaction is conducted for 5 h;
Product treatment: after the reaction ends, an obtained sol- id-liquid mixture is poured into a third beaker for standing and suction filtration, and solid particles are obtained; the obtained solid particles are washed centrifugally for three times with methanol to wash off organic substances left on surfaces of the solid particles, and finally, drying is conducted, until there is no any residual moisture; and the dried solid particles with par- ticle sizes ranging from 120 jm to 250 pm are screened as carbon monoxide gas micro-capsules.
The obtained carbon monoxide gas-sensitive micro-capsules in the embodiment 1 are put into a closed container with a detecting instrument, where the detecting instrument is used for detecting gas volatilized from the limonene;
The gas is introduced into the closed container at a rate of
0.2 L/min; when air is introduced, the gas volatilized from the limonene isn't detected by the detecting instrument, and the rup- ture of the carbon monoxide gas-sensitive micro-capsules doesn't happen; when the carbon monoxide is introduced, the gas volati- lized from the limonene can be detected by the detecting instru- ment within 7.2 min, and the rupture of the carbon monoxide gas- sensitive micro-capsules happens.
Therefore, the carbon monoxide can be detected by the carbon monoxide gas-sensitive micro-capsules in the embodiment 1.
Embodiment 2:
Preparation of a water phase: 0.6g of polyvinyl alcohol is weighed and put into a first beaker, and then, is heated in a thermostat water bath kettle at 80°C, so that it is changed from white granular solids into colorless transparent viscous liquid; and 300ml of distilled water is added into the first beaker, the first beaker is transferred in an ultrasonic cleaner and heated for ultrasonic dissolving for 10 h, until the polyvinyl alcohol is dispersed in water completely and uniformly to form a water phase solution;
Preparation of an organic phase:10g of styrene, 0.5g of divi- nyl benzene, 3g of diisopropyl azodicarboxylate, 0.75g of palladi- um dichloride, and 5 g of limonene are weighed and put into a sec- ond beaker, and then, a mixture is stirred for 3 h with a magnetic stirring apparatus to be mixed fully and uniformly;
A polymerization reaction: a 500 ml flask with three necks is put into a constant temperature oil-bath pan at a temperature of 80°C, the prepared water phase and the organic phase are poured into the 500 ml flask with three necks with stirring, and then, a polymerization reaction is conducted for 5 h;
Product treatment: after the reaction ends, an obtained sol- id-liquid mixture is poured into a third beaker for standing and suction filtration, and solid particles are obtained; the obtained solid particles are washed centrifugally for three times with methanol to wash off organic substances left on surfaces of the solid particles, and finally, drying is conducted, until there is no any residual moisture; and the dried solid particles with par- ticle sizes ranging from 120 um to 250 pm are screened as carbon monoxide gas micro-capsules.
The obtained carbon monoxide gas-sensitive micro-capsules in the embodiment 2 are put into a closed container with a detecting instrument, where the detecting instrument is used for detecting gas volatilized from the limonene;
The gas is introduced into the closed container at a rate of 0.2 L/min; when air is introduced, the gas volatilized from the limonene isn't detected by the detecting instrument, and the rup- ture of the carbon monoxide gas-sensitive micro-capsules doesn't happen; when the carbon monoxide is introduced, the gas volati- lized from the limonene can be detected by the detecting instru- ment within 5.5 min, and the rupture of the carbon monoxide gas- sensitive micro-capsules happens.
Therefore, the carbon monoxide can be detected by the carbon monoxide gas-sensitive micro-capsules in the embodiment 2.
Embodiment 3:
Preparation of a water phase: 0.7g of polyvinyl alcohol is weighed and put into a first beaker, and then, is heated in a thermostat water bath kettle at 80°C, so that it is changed from white granular solids into colorless transparent viscous liquid; and 350ml of distilled water is added into the first beaker, the first beaker is transferred in an ultrasonic cleaner and heated for ultrasonic dissolving for 10 h, until the polyvinyl alcohol is dispersed in water completely and uniformly to form a water phase solution;
Preparation of an organic phase:12g of styrene, 0.6g of divi- nyl benzene, 4g of diisopropyl azodicarboxylate, lg of palladium dichloride, and 5 g of limonene are weighed and put into a second beaker, and then, a mixture is stirred for 3 h with a magnetic stirring apparatus to be mixed fully and uniformly;
A polymerization reaction: a 500 ml flask with three necks is put into a constant temperature oil-bath pan at a temperature of 80°C, the prepared water phase and the organic phase are poured into the 500 ml flask with three necks with stirring, and then, a polymerization reaction is conducted for 5 h;
Product treatment: after the reaction ends, an obtained sol- id-liquid mixture is poured into a third beaker for standing and suction filtration, and solid particles are obtained; the obtained solid particles are washed centrifugally for three times with methanol to wash off organic substances left on surfaces of the solid particles, and finally, drying is conducted, until there is no any residual moisture; and the dried solid particles with par- ticle sizes ranging from 120 pm to 250 pm are screened as carbon monoxide gas micro-capsules.
The obtained carbon monoxide gas-sensitive micro-capsules in the embodiment 3 are put into a closed container with a detecting instrument, where the detecting instrument is used for detecting gas volatilized from the limonene;
The gas is introduced into the closed container at a rate of 0.2 L/min; when air is introduced, the gas volatilized from the limonene isn't detected by the detecting instrument, and the rup- ture of the carbon monoxide gas-sensitive micro-capsules doesn't happen; when the carbon monoxide is introduced, the gas volati- lized from the limonene can be detected by the detecting instru- ment within 4 min, and the rupture of the carbon monoxide gas- sensitive micro-capsules happens.
Therefore, the carbon monoxide can be detected by the carbon monoxide gas-sensitive micro-capsules in the embodiment 3.
The carbon monoxide gas-sensitive micro-capsules that can re- lease corresponding gases are prepared from peppermint oil, men- thol, or other volatile substances that can volatilize non-toxic and harmless gases as core materials by the above method, where the released gases can be detected by the existing gas detector or the existing means (e.g., a gas chromatograph). In addition, if the core materials are solids, it is necessary to add the core ma- terials into the second beaker after being ground.
In the present application, the core materials may be the limonene, the peppermint oil, the menthol, or other volatile sub- stances that can volatilize the non-toxic and harmless gases.
Embodiment 4:
The method for identifying the source of ignition in the worked-out section with the carbon monoxide gas-sensitive micro- capsules includes the following steps:
Step 21: preparing the carbon monoxide gas-sensitive micro-
capsules that can release different gases from different core ma- terials;
At step 22, as a coal face is pushed ahead, areas are divided in a worked-out section at the rear of the coal face, where carbon monoxide gas-sensitive micro-capsules prepared from different core materials are spread; a width of each area is 20 m, as shown in the FIG. 2; in FIG. 2, micro-capsules 1, micro-capsules 2, and mi- cro-capsules 3 are the carbon monoxide gas-sensitive micro- capsules prepared from different core materials, where before be- ing spread in the worked-out section, the carbon monoxide gas- sensitive micro-capsules are stored in high pressure-resistant po- rous balls, as shown in the FIG. 1; the high pressure-resistant porous balls can resist a pressure ranging from 30 MPa to 40 MPa, with an outer diameter ranging from 25,000 um to 45,000 um; and then, the high pressure-resistant porous balls with the carbon monoxide gas-sensitive micro-capsules are spread in different are- as of the worked-out section;
Step 23: arranging a detecting instrument at an upper corner of the coal face, collecting gases in the worked-out section at the upper corner, and detecting gas varieties; and once detecting that the cores containing the carbon monoxide gas-sensitive micro- capsules release gases, giving an alarm immediately;
During coal mining, an air flow of an intake airway of the coal face permeates into the worked-out section at the rear of the coal face from the coal face, and then, returns the coal face from an upper corner, and other areas while carrying gases in the worked-out section, that is, the air flow carrying the gases in the worked-out section will pass through the upper corner of the coal face. Therefore, the gases in the worked-out section can be collected at the upper corner of the coal face.
The collection of the gases can be achieved in the prior art, which will not be described repeatedly herein.
Step 24: determining an area where spontaneous combustion disasters of coals happen in the worked-out section by a worker according to the varieties of the detected core gases.
The carbon monoxide gas-sensitive micro-capsules of the pre- sent disclosure are obtained by suspension polymerization; a wall shell material includes styrene, polyvinyl alcohol, divinyl ben- zene, diisopropyl azodicarboxylate, and palladium dichloride, where the styrene is used as a shell of the wall material, the polyvinyl alcohol is used as a dispersant, the divinyl benzene is used as a cross-linking agent, and the diisopropyl azodicarbox- ylate is used as an initiator; during polymerization, the wall shell material is polymerized into a ball to clad the core materi- als; and the palladium dichloride can react with CO gas. In carbon monoxide environment, wall shells of the gas-sensitive micro- capsules of the present disclosure ruptures due to a reaction be- tween the palladium dichloride and carbon monoxide, releasing the gases volatilized from the core materials. Whether there is the spontaneous combustion of the residual coals can be determined by the detection of the gases of the core materials.
After the carbon monoxide gas-sensitive micro-capsules with different types of core materials are spread in different areas of the worked-out sections, areas where the spontaneous combustion of the residual ccals happens can be determined according to varie- ties of the detected core gases.
The implementations of the present disclosure are described with reference to the drawings, which aren't construed as a limi- tation to the present disclosure. It should understand that vari- ous modifications or variants made by a person skilled in the art on the basis of the technical solutions of the present disclosure, without creative labor, should still be included in the protection scope of the present disclosure.
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| FR2082765A5 (en) * | 1970-03-26 | 1971-12-10 | Commissariat Energie Atomique | |
| SE518522C2 (en) * | 2001-03-21 | 2002-10-22 | Sensistor Ab | Method and device for leakage testing and leak detection |
| JP2006170722A (en) * | 2004-12-14 | 2006-06-29 | Hitachi Chem Co Ltd | Hazardous material sensor unit and sensing system |
| US7670679B2 (en) * | 2006-05-30 | 2010-03-02 | General Electric Company | Core-shell ceramic particulate and method of making |
| EA201490574A1 (en) * | 2011-09-06 | 2014-06-30 | Атонарп Инк. | DEVICE TRACKING FAILURES |
| EP2778657B1 (en) * | 2013-03-15 | 2018-12-12 | Airbus Defence and Space GmbH | Detection device for detecting at least one fault condition |
| CN104418966A (en) * | 2013-09-06 | 2015-03-18 | 广州市香港科大霍英东研究院 | Phase change microcapsule and preparation method thereof |
| CN105080443B (en) * | 2015-08-14 | 2017-07-04 | 佛山市功能高分子材料与精细化学品专业中心 | A kind of microencapsulation material for coating Dicarboxylic Acids and its preparation method and application |
| CN105712393B (en) * | 2016-03-21 | 2017-04-19 | 西北工业大学 | Method for preparing zinc-oxide/simple-substance-carbon core-shell structure |
| CN105924569B (en) * | 2016-05-16 | 2018-05-25 | 昆明理工大学 | A kind of preparation method of multinuclear coated complex microsphere |
| CN106675524B (en) * | 2016-07-13 | 2019-05-17 | 北京化工大学 | A kind of multi-functional phase-change material micro-capsule and preparation method thereof |
| CN109738128B (en) * | 2018-12-29 | 2020-10-02 | 中国矿业大学 | Temperature-sensitive material for predicting spontaneous combustion of coal in goaf, preparation method and application |
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| CN112009859B (en) * | 2020-08-24 | 2022-05-17 | 阿克苏优能农业科技股份有限公司 | Special mould-proof, dust-proof and fresh-keeping net bag for sugar-cored apples and preparation method thereof |
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| CN112362248A (en) * | 2020-10-19 | 2021-02-12 | 太原理工大学 | System and method for detecting goaf air leakage rate under gob-side entry retaining mining in real time |
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