CN108590733A - A kind of preparation method and product of the explosion-suppressing material for inhibiting methane to explode - Google Patents

A kind of preparation method and product of the explosion-suppressing material for inhibiting methane to explode Download PDF

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Publication number
CN108590733A
CN108590733A CN201810385066.5A CN201810385066A CN108590733A CN 108590733 A CN108590733 A CN 108590733A CN 201810385066 A CN201810385066 A CN 201810385066A CN 108590733 A CN108590733 A CN 108590733A
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explosion
attapulgite
suppressing material
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nahco
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CN108590733B (en
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杨克
张平
郝永梅
邢志祥
纪虹
葛云
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Changzhou University
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Changzhou University
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    • EFIXED CONSTRUCTIONS
    • E21EARTH OR ROCK DRILLING; MINING
    • E21FSAFETY DEVICES, TRANSPORT, FILLING-UP, RESCUE, VENTILATION, OR DRAINING IN OR OF MINES OR TUNNELS
    • E21F5/00Means or methods for preventing, binding, depositing, or removing dust; Preventing explosions or fires

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  • Engineering & Computer Science (AREA)
  • Mining & Mineral Resources (AREA)
  • Life Sciences & Earth Sciences (AREA)
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Abstract

The present invention relates to a kind of preparation methods and product of the explosion-suppressing material of inhibition methane explosion, belong to explosion-suppressing material technical field, and this method is by NaHCO3It is particle loaded to the thermal decomposition caloric receptivity of explosion-suppressing material in the high temperature environment on modified attapulgite, is on the one hand improved, on the other hand improve the specific surface area of the material and the dispersion degree in explosion space.The explosion-suppressing material can also handle secondary detonation, because blast wave impact force can again raise the powder to sink, inhibiting effect is played to subsequent explosion flame.The explosion-suppressing material preparation method is simple to operation and at low cost, is suitble to industrialized production.

Description

A kind of preparation method and product of the explosion-suppressing material for inhibiting methane to explode
Technical field
The invention belongs to explosion-suppressing material technical fields, and in particular to a kind of preparation side for the explosion-suppressing material for inhibiting methane to explode Method and product.
Background technology
Coal is the important basic resource in China, in the period of following considerably long in, energy supply based on coal and disappear Expense pattern is difficult to change.Gas is the association product in coal Filling process, based on methane, because methane has combustion when meeting burning things which may cause a fire disaster The possibility burnt and exploded, so gas explosion disaster becomes one of the major casualty for restricting safe coal exploitation.Gas explosion It not only causes a tremendous loss of lives, but also roadway facility can be destroyed, interrupt production, can also cause dust explosion, mine sometimes Fire, roadway such as collapse at the secondary injuries.Therefore, control gas explosion accident is always the main direction of each coal producer's safety of coal mines One of.
Traditional halon fire agent in an atmosphere by solar radiation after, decomposite chlorine, the free radical of bromine seriously destroys Ozone layer;The superfine water mist fire extinguishing system of scholar's research at present, although there is certain progress, but still has deficiency, main to consider Deposit problem both ways:Water mist can be diffused to space wide enough;Sufficiently small and fireballing water particle can be generated.
Therefore, it is badly in need of a kind of explosion-suppressing material environmentally protective, effectiveness of explosion suppression is excellent.
Invention content
In view of this, one of the objects of the present invention is to provide a kind of preparation sides of the explosion-suppressing material of inhibition methane explosion Method;The second purpose is to provide a kind of explosion-suppressing material of inhibition methane explosion.
In order to achieve the above objectives, the present invention provides the following technical solutions:
1, a kind of preparation method for the explosion-suppressing material for inhibiting methane to explode, described method includes following steps:
(1) 140-200 mesh sieve is crossed after drying attapulgite, extracting screen underflow prepares attapulgite suspension, will be described recessed Upper layer solid is taken after convex stick soil suspension centrifugation slagging-off, is pulverized after the upper layer solid is dried, it is recessed after being purified Convex stick soil;
(2) add a concentration of 4-6mol/L's after being added to the water the attapulgite after the purification obtained in step (1) Hydrochloric acid solution stirs 1-2h at 65-85 DEG C, and metal salt solution is made, the attapulgite and hydrochloric acid solution after the purification Mass volume ratio is 1:5-6, the mass volume ratio unit are g:mL;
(3) ammonium hydroxide is added dropwise after metal salt solution obtained in step (2) is cooled to room temperature to the metal salt solution PH value is 7.6-8, forms gel precipitation, adds absolute ethyl alcohol, and 0.5-1h is stirred at 40-50 DEG C, static to place to described Gel precipitation is precipitated completely;
(4) gel precipitation obtained in step (3) is washed with water and is carried out at the same time suction filtration processing, it then will be described It pulverizes after gel precipitation drying, modified attapulgite is made;
(5) the modified attapulgite prepared in step (4) is added in absolute ethyl alcohol, modified concave convex rod is made Native dispersion liquid, then by NaHCO3Solution is added mixing in the modified attapulgite dispersion liquid and obtains mixed liquor, will be described Mixed liquor filters after standing 1-3h, will pulverize after filter residue and drying, and the explosion-suppressing material for inhibiting methane explosion is made;The mixing Modified attapulgite and NaHCO in liquid3Mass ratio be 3-4:5.
Preferably, in step (1), the attapulgite drying is specially:By attapulgite at 60-70 DEG C, infrared striation Dry 8-12h under part, and stir the attapulgite by 12 times/min.
Preferably, in step (1), the speed of the centrifugation is 1300-1500r/min, time 10-15min.
Preferably, in step (1), the upper layer solid drying is specially:The dry 8-12h at 65-85 DEG C;The grinding Time be 2-3h.
Preferably, in step (3), the addition of the absolute ethyl alcohol is equal to the addition of hydrochloric acid solution in step (2).
Preferably, in step (4), the drying is specially:Dry 8-12h, the time of the grinding are at 65-85 DEG C 1-2h。
Preferably, in step (5), modified attapulgite and anhydrous second in the modified attapulgite dispersion liquid The mass volume ratio of alcohol is 3-4:10, the mass volume ratio unit is g:mL.
Preferably, in step (5), the NaHCO3NaHCO in solution3Mass volume ratio with water is 1:10, the quality Volume ratio unit is g:mL.
Preferably, in step (5), the drying is specially:Dry 10-12h, the time of the grinding at 60-70 DEG C For 1-2h.
2, the explosion-suppressing material for inhibiting methane explosion prepared by the method.
The beneficial effects of the present invention are:The present invention provides a kind of preparation methods of the explosion-suppressing material of inhibition methane explosion And product, this method is by NaHCO3It is particle loaded on modified attapulgite, on the one hand improve explosion-suppressing material in high temperature Thermal decomposition caloric receptivity in environment, on the other hand improves the specific surface area of the material and the dispersion degree in explosion space.Wherein, Modified attapulgite inherit the preferable draw ratio of former attapulgite and abundant inner duct and it is non-ignitable the advantages that, it is this more The structure of hole makes it have larger specific surface area and higher surface energy, can not only effectively be adsorbed during datonation-inhibition The living radical generated in explosion reduces living radical concentration, reduces chain reaction activity, forces reaction chain termination, also Toxic volatile ingredient can be absorbed, environmentally protective requirement is reached;In addition, chemical constituent occurs very in modified attapulgite Big to change, the alkali metal ions such as aluminium, magnesium are removed in original ingredient, and the metal oxides such as magnesium, aluminium become metal hydroxides, In hot environment, metal hydroxides can be pyrolyzed water outlet and absorb a large amount of energy, make the explosion-suppressing material finally prepared have compared with High thermal decomposition caloric receptivity, can effectively reduce the temperature of flare system in mine gas explosion.The suppression prepared by this method Quick-fried material can also handle secondary detonation, because blast wave impact force can again raise the powder to sink, to subsequent explosion Flame plays inhibiting effect.The explosion-suppressing material preparation method is simple to operation and at low cost, is suitble to industrialized production.
Description of the drawings
In order to keep the purpose of the present invention, technical solution and advantageous effect clearer, the present invention provides following attached drawing and carries out Explanation:
Fig. 1 is the scanning electron microscope (SEM) photograph of the explosion-suppressing material prepared in embodiment 2;
Fig. 2 is the explosion-suppressing material that the prepares pressure history figure in methane blast process in embodiment 2.
Specific implementation mode
The preferred embodiment of the present invention will be described in detail below.
Embodiment 1
Prepare the explosion-suppressing material for inhibiting methane explosion
(1) by attapulgite at 60 DEG C, dry 12h, during which stirs attapulgite, so by 12 times/min under the conditions of infrared light 140 mesh sieve is crossed afterwards, and extracting screen underflow prepares attapulgite suspension, and attapulgite suspension is centrifuged by the speed of 1300r/min Upper layer solid is taken after 15min slagging-off, upper layer solid is pulverized at 65 DEG C after dry 12h, the time of grinding is 3h, is obtained Attapulgite after purification;
(2) 104mL concentration is added after the attapulgite after the purification obtained in 20g steps (1) being added in distilled water For the hydrochloric acid solution of 6mol/L, 2h is stirred at 85 DEG C, metal salt solution is made;
(3) ammonium hydroxide is added dropwise after metal salt solution obtained in step (2) is cooled to room temperature to the metal salt solution PH value is 7.6, forms gel precipitation, adds the absolute ethyl alcohol isometric with hydrochloric acid solution in step (2), is stirred at 50 DEG C 0.5h, static place to the gel precipitation are precipitated completely;
(4) gel precipitation obtained in step (3) is washed with distilled water and is carried out at the same time suction filtration processing, then will Gel precipitation is pulverized at 65 DEG C after dry 12h, and the time of grinding is 1h, and modified attapulgite is made;
(5) ultrasonic disperse in 40mL absolute ethyl alcohols is added in the modified attapulgite prepared in 12g steps (4) Modified attapulgite dispersion liquid is made, then by 20g NaHCO in 30min3Ultrasound point in 200mL distilled water is added in powder 30min is dissipated, NaHCO is made3Solution, by the NaHCO3Solution is added mixing in the modified attapulgite dispersion liquid and must mix Liquid to be closed, is filtered after which is stood 1h, filter residue is pulverized at 65 DEG C after dry 11h, the time of grinding is 1.5h, The explosion-suppressing material for inhibiting methane explosion is made.
Embodiment 2
Prepare the explosion-suppressing material for inhibiting methane explosion
(1) by attapulgite at 65 DEG C, dry 10h, during which stirs attapulgite, so by 12 times/min under the conditions of infrared light 170 mesh sieve is crossed afterwards, and extracting screen underflow prepares attapulgite suspension, and attapulgite suspension is centrifuged by the speed of 1400r/min Upper layer solid is taken after 12min slagging-off, upper layer solid is pulverized at 70 DEG C after dry 10h, the time of grinding is 2.5h, is obtained Attapulgite after must purifying;
(2) 100mL concentration is added after the attapulgite after the purification obtained in 20g steps (1) being added in distilled water For the hydrochloric acid solution of 5mol/L, 1h is stirred at 65 DEG C, metal salt solution is made;
(3) ammonium hydroxide is added dropwise after metal salt solution obtained in step (2) is cooled to room temperature to the metal salt solution PH value is 8, forms gel precipitation, adds the absolute ethyl alcohol isometric with hydrochloric acid solution in step (2), is stirred at 40 DEG C 1h, static place to the gel precipitation are precipitated completely;
(4) gel precipitation obtained in step (3) is washed with distilled water and is carried out at the same time suction filtration processing, then will Gel precipitation is pulverized at 70 DEG C after dry 10h, and the time of grinding is 1.5h, and modified attapulgite is made;
(5) ultrasonic disperse in 40mL absolute ethyl alcohols is added in the modified attapulgite prepared in 15g steps (4) Modified attapulgite dispersion liquid is made, then by 20g NaHCO in 30min3Ultrasound point in 200mL distilled water is added in powder 30min is dissipated, NaHCO is made3Solution, by the NaHCO3Solution is added mixing in the modified attapulgite dispersion liquid and must mix Liquid is closed, is filtered after which is stood 3h, filter residue is pulverized at 70 DEG C after dry 10h, the time of grinding is 1h, system The explosion-suppressing material that methane must be inhibited to explode.
The explosion-suppressing material prepared in embodiment 2 is scanned by scanning electron microscope, the results are shown in Figure 1, can by Fig. 1 Know, synthesized explosion-suppressing material is in micro- rodlike, and particle size is 20 μm, in addition to this, attached in larger attapulgite particle surface Small crystals, grain size is about 1 μm, thus it is speculated that be the NaHCO for being attached to attapulgite powder body channel surfaces3Crystal.
Embodiment 3
Prepare the explosion-suppressing material for inhibiting methane explosion
(1) by attapulgite at 70 DEG C, dry 8h, during which stirs attapulgite, so by 12 times/min under the conditions of infrared light 200 mesh sieve is crossed afterwards, and extracting screen underflow prepares attapulgite suspension, and attapulgite suspension is centrifuged by the speed of 1500r/min Upper layer solid is taken after 10min slagging-off, upper layer solid is pulverized at 85 DEG C after dry 8h, the time of grinding is 2h, is obtained Attapulgite after purification;
(2) 120mL concentration is added after the attapulgite after the purification obtained in 20g steps (1) being added in distilled water For the hydrochloric acid solution of 4mol/L, 1.5h is stirred at 70 DEG C, metal salt solution is made;
(3) ammonium hydroxide is added dropwise after metal salt solution obtained in step (2) is cooled to room temperature to the metal salt solution PH value is 7.8, forms gel precipitation, adds the absolute ethyl alcohol isometric with hydrochloric acid solution in step (2), is stirred at 45 DEG C 1h, static place to the gel precipitation are precipitated completely;
(4) gel precipitation obtained in step (3) is washed with distilled water and is carried out at the same time suction filtration processing, then will Gel precipitation is pulverized at 85 DEG C after dry 8h, and the time of grinding is 2h, and modified attapulgite is made;
(5) ultrasonic disperse in 40mL absolute ethyl alcohols is added in the modified attapulgite prepared in 16g steps (4) Modified attapulgite dispersion liquid is made, then by 20g NaHCO in 30min3Ultrasound point in 200mL distilled water is added in powder 30min is dissipated, NaHCO is made3Solution, by the NaHCO3Solution is added mixing in the modified attapulgite dispersion liquid and must mix Liquid is closed, is filtered after which is stood 2h, filter residue is pulverized at 60 DEG C after dry 12h, the time of grinding is 2h, system The explosion-suppressing material that methane must be inhibited to explode.
Comparative example 1
Difference lies in do not include step (1)-(4), attapulgite modified in step (5) replaced with embodiment 1 For common concave-convex stick soil.
Comparative example 2
The difference from example 2 is that not including step (1)-(4), attapulgite modified in step (5) is replaced For common concave-convex stick soil.
Comparative example 3
Difference lies in do not include step (1)-(4), attapulgite modified in step (5) replaced with embodiment 3 For common concave-convex stick soil.
By the embodiment 1-3 and comparative example 1-3 explosion-suppressing materials prepared be placed in the environment that methane concentration is 95% into Row is datonation-inhibition, tests the blast pressure value of each explosion-suppressing material, test result is shown in Table 1.
The blast pressure value test result of explosion-suppressing material prepared by 1 embodiment 1-3 of table and comparative example 1-3
Experimental group Comparative example 1 Comparative example 2 Comparative example 3 Embodiment 1 Embodiment 2 Embodiment 3
Blast pressure value 82mbar 68mbar 73mbar 75mbar 61mbar 70mbar
As shown in Table 1, containing the attapulgite modified explosion-suppressing material of equivalent to the effectiveness of explosion suppression of methane be substantially higher in containing There is the explosion-suppressing material of equivalent common concave-convex stick soil.Wherein, in embodiment 1 explosion-suppressing material compared with explosion-suppressing material in comparative example 1, first The blast pressure value of alkane reduces 7mbar;Explosion-suppressing material is compared with explosion-suppressing material in comparative example 2, the explosion pressure of methane in embodiment 2 Force value reduces 7mbar;Explosion-suppressing material is reduced compared with explosion-suppressing material in comparative example 3, the blast pressure value of methane in embodiment 3 3mbar.It can be seen that modified attapulgite is more preferable to the effectiveness of explosion suppression of methane.Wherein, it is prepared in embodiment 2 datonation-inhibition Material is best to the effectiveness of explosion suppression of methane.
By the explosion-suppressing material prepared in embodiment 1-3 and it is attapulgite modified be placed in methane concentration be 95% environment in into Row is datonation-inhibition, tests the blast pressure value of each explosion-suppressing material, test result is shown in Table 2.
As shown in Table 2, simple attapulgite modified explosion-suppressing material and it is compounded with NaHCO3Powder it is attapulgite modified It compares, it is compound by NaHCO3The attapulgite modified explosion-suppressing material of powder is substantially higher in simple the effectiveness of explosion suppression of methane Attapulgite modified explosion-suppressing material.Wherein, the explosion-suppressing material that prepared by embodiment 1 is recessed compared with the simple modification prepared in embodiment 1 The blast pressure value of convex stick soil explosion-suppressing material, methane reduces 21mbar;Explosion-suppressing material prepared by embodiment 2 in embodiment 2 compared with making The blast pressure value of standby simple attapulgite modified explosion-suppressing material, methane reduces 25mbar;Datonation-inhibition material prepared by embodiment 3 Expect that, compared with the simple attapulgite modified explosion-suppressing material prepared in embodiment 3, the blast pressure value of methane reduces 14mbar;Thus As it can be seen that attapulgite modified and NaHCO3The synergistic effect of powder is more preferable to methane effectiveness of explosion suppression.
The explosion-suppressing material prepared in embodiment 2 is added to progress methane explosive test in methane, is in addition implemented with being not added with The methane of the explosion-suppressing material prepared in example 2 explodes check experiment group as methane, test result as shown in Fig. 2, as shown in Figure 2, In addition embodiment 2 after the explosion-suppressing material for preparing, the first peak value and the second peak value of methane explosion decline respectively 1.72kpa and 1.6kpa, while the delay time of the first peak value is 1.6ms, so the addition of the explosion-suppressing material prepared in embodiment 2 is to methane Bursting strength there is apparent datonation-inhibition effect.
Finally illustrate, preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, although logical It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be Various changes are made to it in form and in details, without departing from claims of the present invention limited range.

Claims (10)

1. a kind of preparation method for the explosion-suppressing material for inhibiting methane to explode, which is characterized in that described method includes following steps:
(1) 140-200 mesh sieve is crossed after drying attapulgite, extracting screen underflow prepares attapulgite suspension, by the concave convex rod Upper layer solid is taken after native suspension centrifugation slagging-off, is pulverized after the upper layer solid is dried, the concave convex rod after being purified Soil;
(2) hydrochloric acid of a concentration of 4-6mol/L is added after being added to the water the attapulgite after the purification obtained in step (1) Solution stirs 1-2h at 65-85 DEG C, and metal salt solution, the quality of attapulgite and hydrochloric acid solution after the purification is made Volume ratio is 1:5-6, the mass volume ratio unit are g:mL;
(3) ammonium hydroxide is added dropwise after metal salt solution obtained in step (2) is cooled to room temperature to the pH value of the metal salt solution For 7.6-8, gel precipitation is formed, absolute ethyl alcohol is added, 0.5-1h is stirred at 40-50 DEG C, it is static to place to the gel Precipitation is precipitated completely;
(4) gel precipitation obtained in step (3) is washed with water and is carried out at the same time suction filtration processing, then by the gel It pulverizes after precipitation is dry, modified attapulgite is made;
(5) the modified attapulgite prepared in step (4) is added in absolute ethyl alcohol, modified attapulgite point is made Dispersion liquid, then by NaHCO3Solution is added mixing in the modified attapulgite dispersion liquid and obtains mixed liquor, by the mixing Liquid filters after standing 1-3h, will pulverize after filter residue and drying, and the explosion-suppressing material for inhibiting methane explosion is made;In the mixed liquor Modified attapulgite and NaHCO3Mass ratio be 3-4:5.
2. the method as described in claim 1, which is characterized in that in step (1), the attapulgite drying is specially:It will be recessed Convex stick soil dry 8-12h under the conditions of 60-70 DEG C, infrared light, and stir the attapulgite by 12 times/min.
3. the method as described in claim 1, which is characterized in that in step (1), the speed of the centrifugation is 1300-1500r/ Min, time 10-15min.
4. the method as described in claim 1, which is characterized in that in step (1), the upper layer solid drying is specially:In 65- Dry 8-12h at 85 DEG C;The time of the grinding is 2-3h.
5. the method as described in claim 1, which is characterized in that in step (3), the addition of the absolute ethyl alcohol is equal to step (2) addition of hydrochloric acid solution in.
6. the method as described in claim 1, which is characterized in that in step (4), the drying is specially:It is done at 65-85 DEG C The time of dry 8-12h, the grinding are 1-2h.
7. the method as described in claim 1, which is characterized in that in step (5), in the modified attapulgite dispersion liquid The mass volume ratio of modified attapulgite and absolute ethyl alcohol is 3-4:10, the mass volume ratio unit is g:mL.
8. the method as described in claim 1, which is characterized in that in step (5), the NaHCO3NaHCO in solution3With water Mass volume ratio is 1:10, the mass volume ratio unit is g:mL.
9. the method as described in claim 1, which is characterized in that in step (5), the drying is specially:It is done at 60-70 DEG C The time of dry 10-12h, the grinding are 1-2h.
10. the explosion-suppressing material for inhibiting methane explosion prepared by claim 1-9 any one of them methods.
CN201810385066.5A 2018-04-26 2018-04-26 A kind of preparation method and product of the explosion-suppressing material inhibiting methane explosion Active CN108590733B (en)

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