CN102558763A - Foamable phenolic resin strengthening and filling material for coal mine - Google Patents
Foamable phenolic resin strengthening and filling material for coal mine Download PDFInfo
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Abstract
The invention relates to a foamable phenolic resin strengthening and filling material for coal mine. In the foamable phenolic resin strengthening and filling material for coal mines, a component A is one of inorganic acid and organic acid or a mixture of inorganic acid and organic acid; and a component B is prepared by mixing 90 to 100 weight parts of urea modified phenolic resin with solid content of 65 to 90 weight percent, 6 to 10 weight parts of composite fire retardant, 0 to 15 weight parts of foaming agent, 1 to 5 weight parts of stabilizing agent, 1 to 15 weight parts of cosolvent, 2 to 16 weight parts of antistatic agent and 10 to 30 weight parts of plasticizer, stirring at the temperature of between 30 and 50 DEG C and reacting for 0.5 to 2 hours. When the foamable phenolic resin strengthening and filling material is used, the component A and the component B are mixed and injected into a coal (rock) layer according to the weight ratio of (1-2) : 1 and permeated into small cracks to expand and generate curing reaction for strengthening and sealing the region. According to the foamable phenolic resin strengthening and filling material for coal mines, the compressive strength is more than 40 MPa; the bonding strength is more than or equal to 3.0 MPa; and the foaming coefficient is less than or equal to two times. The foamable phenolic resin strengthening and filling material for coal mines can meet the requirement of coal mine on safety production and can be applied to the industries such as hydroelectric powder, buildings, mining, traffic and the like.
Description
Technical field
The present invention relates to a kind ofly be used for the material that colliery and relevant industries are carried out bonding and reinforcement and filling to coal (rock) body, reinforce and compaction material but more particularly relate to a kind of foamed phenolic resin class.
Background technology
Under action of underground, cofferdam, tunnel, top board, workplace etc. especially loose coal (rock) body very easily collapse and emit, and bring hidden danger to production safety.Particularly, need safeguard exploitation tunnel, chamber, workplace and top board etc. in the process of coal mining along with the popularizing of large-scale fully-mechanized mining equipment.
Slurry injection technique has been widely used in all kinds of geotechnical engineerings since the 1950's.Injecting paste material is divided into cement class and chemical classes material, is respectively applied for different engineering types.The seventies in 20th century, coal-mining technique advanced countries such as Germany, the U.S., the C.I.S., France, Poland have successively developed chemical slip casting material and have been used to reinforce coal and rock and down-hole fireproof, leak stopping wind.Germany, the U.S. are main with polyurethane material, the C.I.S., France, the main urea-formaldehyde resin that uses of Poland.Material year, consumption all effectively improved the resistance to overturning of fractured coal and rock thousands of to more than the ton up to ten thousand, for mine safety and High-efficient Production provide guarantee.
After the seventies in 20th century, along with the fast development of China's Hydraulic and Hydro-Power Engineering, China's ground slurry injection technique also is used widely.Chemical grout has: epoxies, polyurethanes, acrylic amide, formaldehyde resin class, water glass class etc.But above-mentioned materials can not be applied directly to the mine, particularly can not satisfy the needs of colliery downhole production, mainly show as following some.
1, humid environment under the coal mine directly influences the use of the material of surging.
2, the fractured coal and rock after reinforcing will receive once even the repeatedly violent rock pressure [in mine of adopting influences, and the volumetric shrinkage after material is fixed, cohesive strength and ultimate compression strength require height.
3, production safety requirement, the reinforcement material of use must possess high flash point, flame-retarding characteristic.
4, the down-hole airspace is limited, and the objectionable constituent that require material to separate out are strict, in case mine is polluted.
Though 5, downhole crushed coal and rock has crack primary or that mining influence forms, the crack width is little, is difficult to adopt the mineral-type reinforcement material.
6, material should have the rapid hardening characteristic, realizes that chemical consolidation combines with quick propelling of digging construction.
7, in the tunneling process of colliery and stoping operation when running into tomography, can produce inbreak inevitably, and behind frame, form the inbreak hole, often cause methane accumulation, need foam material and carry out filling.
China's coal-mine is employed in methods such as emitting pick-up point frame grillage, back-up sand slurry usually and handles, but these methods are time-consuming, effort, difficulty of construction are big, and can not guarantee really to eliminate accident potential.Therefore, the foam materials that is developed as reinforcing under the coal mine, filling, airtight use is necessary, also will obtain good social benefit and economic benefit.
Summary of the invention
Reinforce and compaction material with the foamed phenolic resin class but the purpose of this invention is to provide a kind of colliery, to satisfy the demand of Safety of Coal Mine Production.
But colliery provided by the invention uses the foamed phenolic resin class to reinforce and compaction material is two-component materials, by separately independently A component and B component form respectively, and the weight ratio of A component and B component is 1～2 ︰ 1.
Particularly, described A component plays solidifying agent, and its composition is one or more the mixture in mineral acid or the organic acid.Wherein, mineral acid is selected from hydrochloric acid, sulfuric acid or phosphoric acid, and organic acid is selected from toluenesulphonic acids, Phenylsulfonic acid or sulfocarbolic acid.
Described B component is a foam material; Urea modified phenolic resin 90～100 weight parts, composite flame-retardant agent 6～10 weight parts, whipping agent 0～15 weight part, stablizer 1～15 weight part, solubility promoter 1～15 weight part, static inhibitor 2～16 weight parts, softening agent 10～30 weight parts by solid content 65～90wt% mix, and obtain in 0.5～2 hour at 30～50 ℃ of stirring reactions.
In the above-mentioned B component; Described composite flame-retardant agent is to be composited by inorganic combustion inhibitor and the organic fire-retardant weight ratio according to 1 ︰ 2～5; Wherein, Described inorganic combustion inhibitor is Marinco H or white lake, and perhaps their mixture, organic fire-retardant are a kind of in three (β-chloroethyl) SULPHOSUCCINIC ACID ESTER (TCEP), tricresyl phosphate (2-chloropropyl) ester (TCPP), the dimethyl methyl phosphonate (DMMP) or their mixture.
Described whipping agent uses pneumatogen, like methylene dichloride, CFCs class or their mixture.
Described stablizer is the equal infusion of organic silicone oil, or Tweens, perhaps their mixture.
Usually, the static inhibitor of adding is cationic static inhibitor, preferred long chain alkyl ammonium salt class static inhibitor.
The preferred phthalic easter plastizer of softening agent of the present invention is like Witcizer 300, diisobutyl phthalate etc.
The solubility promoter that the present invention uses is terepthaloyl moietie.
It is emphasized that urea modified phenolic resin of the present invention is earlier under basic catalyst, phenol and Paraformaldehyde 96 carry out polyreaction, add the urea continuation again and react the urea modified phenolic resin that obtains.
Concrete, be in the presence of basic catalyst, earlier phenol and Paraformaldehyde 96 are obtained resol 80～95 ℃ of polyreactions, add urea again, continue reaction in 80～85 ℃ and obtain urea modified phenolic resin.Wherein, the consumption of basic catalyst is 1～2% of a phenol weight, and the mol ratio of phenol, Paraformaldehyde 96, urea satisfies 1 ︰, 1.5～2.2 ︰ 4.5～6.5.
In the aforesaid method, described basic catalyst is a kind of or any two kinds mixture in sodium hydroxide, Pottasium Hydroxide, hydrated barta, ammoniacal liquor, yellow soda ash, the zinc acetate.
What the present invention used is the urea modified phenolic resin of solid content 65～90wt%, is the above-mentioned urea modified phenolic resin for preparing to be added water dilute, and 65～90wt% obtains to the urea modified phenolic resin solid content.
But colliery of the present invention reinforces with the foamed phenolic resin class and the method for use of compaction material is; With pump A component and B component are mixed pressure injection coal (rock) layer according to the weight ratio of 1～2 ︰ 1; Be penetrated into fine cracks and expand, curing reaction takes place, thereby reinforce effectively and the encapsulation process zone.
Described pump can adopt the two fluid grouting pump, wherein, under the colliery, uses air-driven type two fluid grouting pump, uses power type two fluid grouting pump at elswhere.
But colliery provided by the invention has solved the problem of existing resol embrittlement with reinforcing of foamed phenolic resin class and compaction material; Make reinforcement material and compaction material can satisfy the actual needs of Safety of Coal Mine Production, and can be used for industries such as water power, building, mining and traffic.
Beneficial effect of the present invention is mainly reflected in following aspect.
1, material of the present invention is used for Safety of Coal Mine Production, for mine safety and High-efficient Production provide guarantee.
2, material of the present invention has been realized foaming at normal temp curing, adjustable curing speed, and cured body intensity is high; The ultimate compression strength of polymkeric substance has extremely strong cohesive strength, cohesive strength>=3.0MPa under the equal rate of expansion condition after the curing more than 40MPa; When using as reinforcement material, foaming coefficient≤2 times.
3, material slurries calculus rate of the present invention is high, does not chap, and adapts to the distortion of reinforcing back coal (rock) body, has certain snappiness, tensile strength >=10MPa.
4, material perviousness of the present invention is strong, and good fluidity can penetrate into the fine gap of coal (rock) body, and foam expansion can be adjusted; Material is fire-retardant, antistatic effect satisfies underground mine use polymer product MT113-1995 technological standard.
5, the production process of material of the present invention and product fraction and polymkeric substance are nontoxic, and be harmless, pollution-free, compliance with environmental protection requirements.
6, material of the present invention also can be used for the reinforcing and the filling of industries such as water power, building, mining and traffic.
Embodiment
Embodiment 1.
Consisting of of A component solidifying agent: toluenesulphonic acids 85Kg, Phenylsulfonic acid 15Kg, phosphatase 11 00Kg, dissolving mixes subsequent use.
Take by weighing in 30%KOH solution 15Kg, the fused phenol 400Kg adding reaction kettle; During heated and stirred to 75 ℃; Begin to add Paraformaldehyde 96, under 80～85 ℃ of temperature, in 1 hour, the 250Kg Paraformaldehyde 96 is divided in six adding reaction kettles, after adding; In 30 minutes, be warmed up to 95 ℃, and under this temperature insulation reaction 20 minutes.Add urea 80Kg again, 85 ℃ of insulation reaction 30 minutes.Add the dilution of 100Kg water at last and stir, obtain the urea modified phenolic resin of solid content 86.92%.
Get the urea modified phenolic resin 100Kg of the above-mentioned solid content for preparing 86.92%; Be cooled to 60 ℃, add 5Kg DMMP, 1.25Kg white lake, 10Kg tween-80 and 10Kg terepthaloyl moietie successively, mix; Continue to be cooled to 40 ℃; Add methylene dichloride 2.5Kg, dodecyl benzyl dimethyl ammonium chloride 5Kg, diisobutyl phthalate 10Kg mix, and continue stirring and obtain B component foam material in 1 hour.
A component and B component is mixing cured according to the weight ratio of 1 ︰ 1 through the two fluid grouting pump, detect its performance, 1.5 times of foam expansion; Ultimate compression strength 40MPa; Tensile strength 15.6MPa, cohesive strength 3.3MPa, flame retardant properties: it is that 0s, smokeless combustion time are 1.7s that the blowtorch method has cigarette combustion time; It is that 0s, smokeless combustion time are 2.5s that the spirit lamp method has cigarette combustion time, meets the MT113-1995 technological standard.
Embodiment 2.
Consisting of of A component solidifying agent: toluenesulphonic acids 85Kg, Phenylsulfonic acid 15Kg, hydrochloric acid 70Kg, dissolving mixes subsequent use.
Take by weighing in 30%NaOH solution 19.25Kg, the fused phenol 385Kg adding reaction kettle; Begin to add Paraformaldehyde 96 200Kg during heated and stirred to 78 ℃, remain temperature at 80～85 ℃ in the reinforced process, after adding; In 30 minutes, be warmed up to 95 ℃, insulation reaction is 20 minutes under this temperature.Add urea 65Kg again, 85 ℃ of insulation reaction 30 minutes.Add the dilution of 300Kg water at last and stir, obtain the urea modified phenolic resin of solid content 67.66%.
Get the urea modified phenolic resin 100Kg of the above-mentioned solid content for preparing 67.66%; Be cooled to 65 ℃, add 5Kg TCEP, 1.25Kg Marinco H, 10Kg tween-80 and 10Kg terepthaloyl moietie successively, mix; Continue to be cooled to 35 ℃; Add CFCs HCFC-141b 4.5Kg, DTAC 5Kg, Witcizer 300 15Kg mix, and continue stirring and obtain B component foam material in 1.5 hours.
A component and B component is mixing cured according to the weight ratio of 1 ︰ 1 through the two fluid grouting pump, detect its performance, 1.5 times of foam expansion; Ultimate compression strength 48MPa; Tensile strength 16.9MPa, cohesive strength 3.5MPa, flame retardant properties: it is that 0s, smokeless combustion time are 1.9s that the blowtorch method has cigarette combustion time; It is that 0s, smokeless combustion time are 2.8s that the spirit lamp method has cigarette combustion time, meets the MT113-1995 technological standard.
Embodiment 3.
Consisting of of A component solidifying agent: toluenesulphonic acids 85Kg, sulfuric acid 3Kg, phosphatase 11 00Kg, dissolving mixes subsequent use.
Take by weighing in 30%KOH solution 23Kg, the fused phenol 350Kg adding reaction kettle; Begin to add Paraformaldehyde 96 during heated and stirred to 75 ℃; Maintain the temperature at 80～85 ℃ in the reinforced process; In 1 hour, add the 200Kg Paraformaldehyde 96 several times, in 30 minutes, be warmed up to 95 ℃ of insulation reaction 20 minutes afterwards.Add urea 72Kg again, 85 ℃ of insulation reaction 30 minutes.Add the dilution of 200Kg water at last and stir, obtain the urea modified phenolic resin of solid content 74.21%.
Get the urea modified phenolic resin 100Kg of the above-mentioned solid content for preparing 74.21%; Be cooled to 60 ℃, add 5Kg DMMP, 1.25Kg Marinco H, the equal infusion AK-158 of 10Kg organic silicone oil and 10Kg terepthaloyl moietie successively, mix; Continue to be cooled to 35 ℃; Add methylene dichloride 12Kg, dodecyl benzyl dimethyl ammonium chloride 10Kg, diisobutyl phthalate 5Kg mix, and continue stirring and obtain B component foam material in 2 hours.
A component and B component is mixing cured according to the weight ratio of 1 ︰ 1 through the two fluid grouting pump, detect its performance, 30 times of foam expansion, ultimate compression strength 1.4MPa, flame retardant properties: it is that 0s, smokeless combustion time are 2.5s that the blowtorch method has cigarette combustion time; It is that 0s, smokeless combustion time are 3.6s that the spirit lamp method has cigarette combustion time, meets the MT113-1995 technological standard.
Embodiment 4.
Consisting of of A component solidifying agent: toluenesulphonic acids 95Kg, Phenylsulfonic acid 25Kg, phosphoric acid 75Kg, dissolving mixes subsequent use.
Take by weighing in 30%KOH solution 20Kg, the fused phenol 400Kg adding reaction kettle; Begin to add Paraformaldehyde 96 during heated and stirred to 75 ℃; Maintain the temperature at 80～85 ℃ in the reinforced process, in 1 hour, add the 225Kg Paraformaldehyde 96, be warming up to 95 ℃ of insulation reaction afterwards 30 minutes.Add urea 82Kg again, 85 ℃ of insulation reaction 30 minutes.Add the dilution of 100Kg water at last and stir, obtain the urea modified phenolic resin of solid content 85.93%.
Get the urea modified phenolic resin 100Kg of the above-mentioned solid content for preparing 85.93%; Be cooled to 55 ℃; Add 7Kg TCPP, 1.25Kg Marinco H, the equal infusion AK-158 of 5Kg organic silicone oil, 2Kg tween-80 and 10Kg terepthaloyl moietie successively; Mix, continue to be cooled to 30 ℃, add CFCs HCFC-141b 2.5Kg, methylene dichloride 1.5Kg; Dodecyl benzyl dimethyl ammonium chloride 5Kg, Witcizer 300 15Kg mix, and continue stirring and obtain B component foam material in 1.5 hours.
A component and B component is mixing cured according to the weight ratio of 1 ︰ 1 through the two fluid grouting pump, detect its performance, 1 times of foam expansion; Ultimate compression strength 45MPa; Tensile strength 19.1MPa, cohesive strength 4.0MPa, flame retardant properties: it is that 0s, smokeless combustion time are 1.8s that the blowtorch method has cigarette combustion time; It is that 0s, smokeless combustion time are 2.7s that the spirit lamp method has cigarette combustion time, meets the MT113-1995 technological standard.
Embodiment 5.
Consisting of of A component solidifying agent: hydrochloric acid 35Kg, Phenylsulfonic acid 15Kg, phosphoric acid 85Kg, dissolving mixes subsequent use.
Take by weighing in 30%NaOH solution 16Kg, the fused phenol 400Kg adding reaction kettle; Begin to add Paraformaldehyde 96 during heated and stirred to 75 ℃; The 200Kg Paraformaldehyde 96 was divided in 1 hour in six adding reaction kettles; Maintain the temperature at 80～85 ℃ in the reinforced process, in 20 minutes, be warming up to 95 ℃ afterwards, insulation reaction 20 minutes.Add urea 80Kg again, 80 ℃ of insulation reaction 35 minutes.Add the dilution of 150Kg water at last and stir, obtain the urea modified phenolic resin of solid content 80.95%.
Get the urea modified phenolic resin 100Kg of the above-mentioned solid content for preparing 80.95%; Be cooled to 60 ℃; Add 6Kg TCEP, 2Kg TCPP, 2Kg white lake, the equal infusion AK-158 of 10Kg organic silicone oil and 10Kg terepthaloyl moietie successively, mix, continue to be cooled to 35 ℃; Adding DTAC 5Kg, Witcizer 300 10Kg mix, and continue stirring and obtain B component foam material in 0.5 hour.
A component and B component is mixing cured according to the weight ratio of 1 ︰ 1 through the two fluid grouting pump, detect its performance, 1.2 times of foam expansion; Ultimate compression strength 53MPa; Tensile strength 18.6MPa, cohesive strength 4.3MPa, flame retardant properties: it is that 0s, smokeless combustion time are 1.5s that the blowtorch method has cigarette combustion time; It is that 0s, smokeless combustion time are 2.8s that the spirit lamp method has cigarette combustion time, meets the MT113-1995 technological standard.
More than each embodiment only be used for the explanation that makes an explanation to the present invention; Do not constitute qualification to the claim scope; Those skilled in the art's other alternative means that description can be expected according to the present invention all should be within the protection domain of claim of the present invention.
Claims (10)
1. but a colliery reinforces and compaction material with the foamed phenolic resin class, it is characterized in that by separately independently A component and B component form, and the weight ratio of A component and B component is 1～2 ︰ 1,
Described A component is a solidifying agent, is one or more the mixture in mineral acid or the organic acid;
Described B component is a foam material; Urea modified phenolic resin 90～100 weight parts, composite flame-retardant agent 6～10 weight parts, whipping agent 0～15 weight part, stablizer 1～5 weight part, solubility promoter 1～15 weight part, static inhibitor 2～16 weight parts, softening agent 10～30 weight parts by solid content 65～90wt% mix, and obtain in 0.5～2 hour at 30～50 ℃ of stirring reactions;
Wherein, described urea modified phenolic resin is in the presence of basic catalyst, and phenol and Paraformaldehyde 96 polyreaction obtain resol, adds urea continuation reaction again and obtains urea modified phenolic resin.
2. but colliery according to claim 1 reinforces and compaction material with the foamed phenolic resin class; It is characterized in that described urea modified phenolic resin is in the presence of basic catalyst; Phenol and Paraformaldehyde 96 are obtained resol 80～95 ℃ of polyreactions; Add urea again, continue reaction in 80～85 ℃ and obtain urea modified phenolic resin, wherein; The consumption of basic catalyst is 1～2% of a phenol weight, and the mol ratio of phenol, Paraformaldehyde 96, urea satisfies 1 ︰, 1.5～2.2 ︰ 4.5～6.5.
3. but colliery according to claim 1 and 2 reinforces and compaction material with the foamed phenolic resin class, it is characterized in that described basic catalyst is a kind of or any two kinds mixture in sodium hydroxide, Pottasium Hydroxide, hydrated barta, ammoniacal liquor, yellow soda ash, the zinc acetate.
4. but colliery according to claim 1 reinforces and compaction material with the foamed phenolic resin class, it is characterized in that described mineral acid is hydrochloric acid, sulfuric acid or phosphoric acid.
5. but colliery according to claim 1 reinforces and compaction material with the foamed phenolic resin class, it is characterized in that described organic acid is toluenesulphonic acids, Phenylsulfonic acid or sulfocarbolic acid.
6. but colliery according to claim 1 reinforces and compaction material with the foamed phenolic resin class; It is characterized in that described composite flame-retardant agent is composited by inorganic combustion inhibitor and the organic fire-retardant weight ratio according to 1 ︰ 2～5; Inorganic combustion inhibitor wherein is Marinco H or white lake; Perhaps their mixture, organic fire-retardant are a kind of in three (β-chloroethyl) SULPHOSUCCINIC ACID ESTER, tricresyl phosphate (2-chloropropyl) ester, the dimethyl methyl phosphonate or their mixture.
7. but colliery according to claim 1 reinforces and compaction material with the foamed phenolic resin class, it is characterized in that described whipping agent is pneumatogen methylene dichloride, CFCs class or their mixture.
8. but colliery according to claim 1 is characterized in that with foamed phenolic resin class reinforcing and compaction material and method for making thereof described stablizer is the equal infusion of organic silicone oil, or Tweens, perhaps their mixture.
9. but claim 1 colliery is characterized in that with pump A component and B component being mixed pressure injection coal rock layer according to the weight ratio of 1～2 ︰ 1 with the method for use of reinforcing of foamed phenolic resin class and compaction material, is penetrated into fine cracks and expands, the generation curing reaction.
10. but colliery according to claim 9 reinforces with the foamed phenolic resin class and the method for use of compaction material, it is characterized in that described pump adopts the two fluid grouting pump.
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| CN104558477A (en) * | 2014-12-26 | 2015-04-29 | 北京瑞诺安科新能源技术有限公司 | Silicate modified polyurethane foam material, as well as preparation method and application method thereof |
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