CN103333668A - Permeable water plugging modified phenolic resin injecting paste material for underground coal mine and preparation method - Google Patents
Permeable water plugging modified phenolic resin injecting paste material for underground coal mine and preparation method Download PDFInfo
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- CN103333668A CN103333668A CN2013103079434A CN201310307943A CN103333668A CN 103333668 A CN103333668 A CN 103333668A CN 2013103079434 A CN2013103079434 A CN 2013103079434A CN 201310307943 A CN201310307943 A CN 201310307943A CN 103333668 A CN103333668 A CN 103333668A
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Abstract
The invention discloses a permeable water plugging modified phenolic resin injecting paste material for an underground coal mine and a preparation method and aims to solve the problem that a water plugging effect is not ideal by adopting a traditional material. The preparation method is characterized by comprising the following steps of preparing a component A from phenol, formaldehyde, barium hydroxide, oxalic acid and urea, preparing a component B from phenolsulfonic acid, phosphoric acid and para-toluenesulfonic acid, and then, mixing the component A and the component B in weight ratio of 1:1. The material disclosed by the invention is low in viscosity and high in liquidity and is capable of completely plugging ultra-thin cracks, is high in curing time which is adjustable on site within a range of 5-60 seconds; a polymer cannot be pulverized, is stable when meeting water and is capable of permanently plugging the cracks. The material reaches a fire-retardant level and is environmentally friendly; production raw materials are completely domesticated and are pollution-free; the construction is simple; the operation is simple and easy to implement; the environment cannot be polluted during a production process, and the health of workers is not influenced.
Description
Technical field
The present invention relates to a kind of underground mine use seepage water shutoff material, relate to a kind of modified phenolic resins injecting paste material or rather.
Background technology
In the middle of process of coal mining, because the variation of geology, it is broken that coal rock layer produces fracture, enriching local water sees through among the inflow tunnel, broken crack, not only make troubles to safety in production, and along with current wash away for a long time, space, coal petrography crack constantly increases, situation such as also may cause roof fall, subside impacts for miner's life.
Methods such as guiding, extraction and injection chemical pulp have mainly been taked to the improvement of water under the down-hole in the colliery.Guiding and extraction can not fundamentally solve the situation of leaking, and existing grouting method mainly is to use urethane perforating slip casting is carried out in the zone that leaks, and the quick-setting characteristics of handy urethane are carried out shutoff to the coal petrography crack, to reach the effect of water blockoff.
But polyurethane material is too strong to the reaction of water in the middle of polymerization process, mainly show meet water sharply foaming be split into hollow, can't bear permanent hydraulic pressure, water plugging effect is undesirable, particularly at home at 10m per hour
3Under the situation of discharge, adopt the method for guiding, extraction to guarantee downhole safety production mostly.
Summary of the invention
The invention provides a kind of underground mine use seepage water blockoff modified phenolic resins injecting paste material, can be applicable to fully that aquifer yield is at 30 m
3/ hour with interior zone, permanent leak stopping, and can play reinforcement effect, material reaches difficult combustion level, and is indeformable, stability is high, and the pressure height is shock-resistant, is universally acknowledged environment-friendly materials, pollution-free, construction is simple, and is not high to personnel and equipment requirements, can satisfy the effect of colliery water blockoff fully.
The present invention also provides a kind of preparation method of underground mine use seepage water blockoff modified phenolic resins injecting paste material, and starting material domesticize fully, and are with short production cycle, low to personnel and equipment requirements.
Underground mine use seepage water blockoff modified phenolic resins injecting paste material of the present invention is characterized in that being mixed and made into by A component and B component, by weight the A component: B component=1:1;
Described A component raw material is made by following raw material according to the parts by weight meter:
20-40 parts of phenol, 60-70 parts in formaldehyde, 3-6 parts of hydrated bartas, 1-1.5 parts of oxalic acid, 5-10 parts in urea;
Described B component starting material are made by following raw material according to the parts by weight meter:
40-80 parts of sulfocarbolic acids, 0-40 parts of phosphatase 11s, 10-40 parts of tosic acid.
Desired raw material is the commercially available prod in the wherein said A component, and phenol content more than 99%, formaldehyde content 37 ± 1%, hydrated barta are 8 water hydrated bartas, oxalic acid content 〉=99.6%, urea nitrogen content 47 ± 1%;
Desired raw material is the commercially available prod in the wherein said B component, sulfocarbolic acid content 65 ± 2%, phosphorus acid content 99 ± 2%, tosic acid content 80 ± 2%.
The preparation method of underground mine use seepage water blockoff modified phenolic resins injecting paste material of the present invention is characterized in that preparing respectively A component, B component, and again according to the A component: the weight ratio of B component=1:1 is mixed;
The preparation method of described A component comprises following concrete steps:
Formaldehyde, phenol, the hydrated barta of standard metering are dropped in the reactor, when temperature rises to 40-45
0Stop indirect heating during C, be warming up to 65-70 automatically
0Be incubated during C, when the emulsification point reaches 20-40ml, add oxalic acid, when PH reaches 7-8, add the urea dehydration again, when viscosity reaches 40-80mpa ﹒ s(25
0C), stop going up dehydration, sampling Detection, qualified back blowing packs;
The preparation method of described B component comprises following concrete steps:
Benzaldehyde sulfonic acid, phosphoric acid, the tosic acid of standard metering are dropped in the stirred pot, stir, sampling in 30 minutes detects, and viscosity is at 10-30 mpa ﹒ s(25
0C), qualified back blowing packs.
Underground mine use seepage water blockoff modified phenolic resins injecting paste material of the present invention is in use according to the A component: the weight ratio of B component=1:1 is mixed, with pneumatic two fluid grouting infusion regional the getting final product of going into to leak.
The present invention compared with prior art has following beneficial effect:
Material viscosity is low, A component 40-80mpa ﹒ s(25
0C), B component 10-30 mpa ﹒ s(25
0C), mobile strong, fully can the superfine crack of shutoff, set time is fast, and 5-60 seconds are on-the-spot adjustable, not efflorescence of polymer, it is stable to meet water, permanent leak stopping, material reaches difficult combustion level environment-friendly materials, and raw materials for production domesticize fully, and are pollution-free; Construction is simple, and operation is simple; Environmentally safe in the production process does not influence the healthy of workman.
Embodiment
The invention will be further described below in conjunction with case study on implementation.
Embodiment one:
The preparation of A component
In 4 parts of input reactors of 60 parts in 30 parts of phenol, formaldehyde, hydrated barta with standard metering, heat to 40
0C heats on stopping, and is warmed up to 70 automatically
0C insulation detects every sampling in 30 minutes, when emulsification during o'clock to 25-35ml, adds 1 part of neutralization of oxalic acid, adds 5 parts of urea dehydrations when PH to 7-8, detect every sampling in 30 minutes, when viscosity at 40-80 mpa ﹒ s(25
0C) time, resampling detects, and qualified blowing packs;
The preparation of B component
With 40 parts of sulfocarbolic acids, 0 part of the phosphatase 24 of standard metering, tosic acid drops into stirred pot for 20 parts and stirs, and sampling detects after 30 minutes, and qualified back blowing packs.
The testing product index is as follows:
Viscosity 25
0C A component 60 mpa ﹒ s B components 25 mpa ﹒ s
Proportion A component 1.17 kg/cm
3B component 1.26kg/cm
3
Set time (25
0C) 15 seconds
Temperature of reaction (25
0C) 75
0C
Expansion multiple 1
Ultimate compression strength 26mpa
Water blockoff amount 20m
3/ hour
Oxygen index 47.5
During use according to the A component: B components by weight 1:1, mix into polymer, with pneumatic two fluid grouting infusion go into to leak the zone get final product.
Embodiment two:
The preparation of A component
During 65 parts in standard metering formaldehyde, 25 parts of phenol, 5 parts of input reactors of hydrated barta are gone into, heat to material temperature 40
0C stops to heat, and is warmed up to 65 automatically
0Be incubated during C, detect every sampling in 30 minutes.When the emulsification point reaches between 35-40ml, add 1.2 parts of neutralizations of oxalic acid, when pH value to 7-8, dewater after adding 3.8 parts of urea, every sampling detection in 30 minutes, as viscosity 40-80 mpa ﹒ s(25
0C) time, sampling detects, and qualified back blowing packs;
The preparation of B component
20 parts of inputs of 20 parts of 60 parts of sulfocarbolic acids, phosphoric acid, tosic acid stirred pot of standard metering is stirred, and sampling detects after 30 minutes, and qualified back blowing packs.
The testing product index is as follows:
Viscosity A component 70 mpa ﹒ s B components 28 mpa ﹒ s
Proportion A component 1.20 kg/cm
3B component 1.20 kg/cm
3
Set time (25
0C) 10s
Temperature of reaction 78
0C
Expansion multiple 1
Water blockoff amount 25m
3/ hour
Oxygen index 47.5
During use according to the A component: the weight ratio of B component, mix into polymer, with pneumatic two fluid grouting infusion go into to leak the zone get final product.
Embodiment three
The preparation of A component
During 6 parts of input reactors of 22 parts of 64 parts in formaldehyde, phenol, hydrated barta of standard metering are gone into, heat to material temperature 40
0C stops heating, is warming up to 65 automatically
0Be incubated during C, detect every sampling in 30 minutes.When the emulsification point reaches 35-40ml, add 1.5 parts of neutralizations of oxalic acid, when pH value to 7-8, add 6.5 parts of urea dehydrations, detect every sampling in 30 minutes, when viscosity at 40-80 mpa ﹒ s(25
0C) time, resampling detects, and packs after qualified;
The preparation of B component
With 80 parts of standard metering sulfocarbolic acids, 0 part of phosphatase 11, tosic acid drops into stirred pot for 10 parts and stirs, and sampling detects after 30 minutes, and qualified back blowing packs.
The testing product index is as follows:
Viscosity A component 75 mpa ﹒ s B components 30 mpa ﹒ s
Proportion A component 1.21 kg/cm
3B component 1.25 kg/cm
3
Set time (25
0C) 7s
Temperature of reaction (25
0C) 82
0C
Expansion multiple 1
Water blockoff amount 30m
3/ hour
Oxygen index 47.5
During use according to the A component: the weight ratio of B component 1:1, mix into polymer, go into to get final product with qigong two fluid grouting infusion.
Claims (2)
1. a underground mine use seepage water blockoff modified phenolic resins injecting paste material is characterized in that being mixed and made into by A component and B component, by weight the A component: B component=1:1;
Described A component raw material is made by following raw material according to the parts by weight meter:
20-40 parts of phenol, 60-70 parts in formaldehyde, 3-6 parts of hydrated bartas, 1-1.5 parts of oxalic acid, 5-10 parts in urea;
Described B component starting material are made by following raw material according to the parts by weight meter:
40-80 parts of sulfocarbolic acids, 0-40 parts of phosphatase 11s, 10-40 parts of tosic acid.
2. the preparation method of a underground mine use seepage water blockoff modified phenolic resins injecting paste material is characterized in that preparing respectively A component, B component, and again according to the A component: the weight ratio of B component=1:1 is mixed;
The preparation method of described A component comprises following concrete steps:
Formaldehyde, phenol, the hydrated barta of standard metering are dropped in the reactor, when temperature rises to 40-45
0Stop indirect heating during C, be warming up to 65-70 automatically
0Be incubated during C, when the emulsification point reaches 20-40ml, add oxalic acid, when PH reaches 7-8, add the urea dehydration again, when viscosity reaches 40-80mpa ﹒ s(25
0C), stop going up dehydration, sampling Detection, qualified back blowing packs;
The preparation method of described B component comprises following concrete steps:
Benzaldehyde sulfonic acid, phosphoric acid, the tosic acid of standard metering are dropped in the stirred pot, stir, sampling in 30 minutes detects, and viscosity is at 10-30mpa ﹒ s(25
0C), qualified back blowing packs.
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| CN201310307943.4A CN103333668B (en) | 2013-07-22 | 2013-07-22 | Underground mine use seepage water blockoff modified phenolic resins injecting paste material and preparation method |
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| CN103333668B CN103333668B (en) | 2015-11-04 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103740348A (en) * | 2013-12-31 | 2014-04-23 | 东营泰尔石油技术有限公司 | Leaking stoppage reinforcing agent |
| CN104479664A (en) * | 2014-11-19 | 2015-04-01 | 长江大学 | Organic granular plugging agent for CO2-driving high-temperature low-permeation water-sensitive oil deposit and preparation method thereof |
| CN106047319A (en) * | 2016-06-08 | 2016-10-26 | 唐山市金沙工贸有限公司 | Blocking agent for pressurized operation tube string for oil and gas field development and blocking technology adopting blocking agent |
| CN107151415A (en) * | 2017-06-13 | 2017-09-12 | 张子光 | Engineering water blockoff phenolic resin injecting paste material and preparation method |
| CN108997987A (en) * | 2018-07-16 | 2018-12-14 | 唐山市金沙工贸有限公司 | A kind of oil-gas field development Operating Pressure tubing string sealing agent and preparation method thereof |
| CN110358249A (en) * | 2019-06-21 | 2019-10-22 | 中煤第五建设有限公司 | Low aldehyde type modified urea-formaldehyde resin grouting for water blocking material of a kind of environmental protection and preparation method thereof |
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| CN101781393A (en) * | 2009-01-19 | 2010-07-21 | 济南圣泉集团股份有限公司 | Resin for high-flame-retardant phenol formaldehyde foam and production method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103740348A (en) * | 2013-12-31 | 2014-04-23 | 东营泰尔石油技术有限公司 | Leaking stoppage reinforcing agent |
| CN104479664A (en) * | 2014-11-19 | 2015-04-01 | 长江大学 | Organic granular plugging agent for CO2-driving high-temperature low-permeation water-sensitive oil deposit and preparation method thereof |
| CN106047319A (en) * | 2016-06-08 | 2016-10-26 | 唐山市金沙工贸有限公司 | Blocking agent for pressurized operation tube string for oil and gas field development and blocking technology adopting blocking agent |
| CN107151415A (en) * | 2017-06-13 | 2017-09-12 | 张子光 | Engineering water blockoff phenolic resin injecting paste material and preparation method |
| CN108997987A (en) * | 2018-07-16 | 2018-12-14 | 唐山市金沙工贸有限公司 | A kind of oil-gas field development Operating Pressure tubing string sealing agent and preparation method thereof |
| CN110358249A (en) * | 2019-06-21 | 2019-10-22 | 中煤第五建设有限公司 | Low aldehyde type modified urea-formaldehyde resin grouting for water blocking material of a kind of environmental protection and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN103333668B (en) | 2015-11-04 |
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Effective date of registration: 20181127 Address after: 235000 Shitai Town, Duji District, Huaibei City, Anhui Province Patentee after: HUAIBEI WANYUAN INDUSTRY TRADE Co.,Ltd. Address before: 235052 Shuoli Town, Huaibei City, Anhui Province, Huaibei Baihui Industry and Trade Co., Ltd. Patentee before: Huaibei Baihui Industry and Trade Co.,Ltd. |
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Granted publication date: 20151104 Termination date: 20210722 |