CN104016613B - A kind ofly improve additive of filling in mine slip degree of mobilization and preparation method thereof - Google Patents

A kind ofly improve additive of filling in mine slip degree of mobilization and preparation method thereof Download PDF

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Publication number
CN104016613B
CN104016613B CN201410275390.3A CN201410275390A CN104016613B CN 104016613 B CN104016613 B CN 104016613B CN 201410275390 A CN201410275390 A CN 201410275390A CN 104016613 B CN104016613 B CN 104016613B
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additive
reaction
mobilization
filling
preparation
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CN104016613A (en
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周爱民
宋嘉栋
张友轩
宋兴
袁雪梅
王长军
詹进
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Changsha Institute of Mining Research Co Ltd
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Changsha Institute of Mining Research Co Ltd
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  • Soil Conditioners And Soil-Stabilizing Materials (AREA)

Abstract

The present invention relates to and a kind ofly improve additive of filling in mine slip degree of mobilization and preparation method thereof, be prepared from by following raw materials according by weight percentage: beta-naphthalenesulfonic-acid salt formaldehyde condensation products 35% ~ 45%, polyvinyl alcohol 2% ~ 5%, calglucon 4% ~ 10%, Tai-Ace S 150 1% ~ 2%, citric acid 15% ~ 18%, water 20% ~ 42%.Additive of the present invention can meet mobility and early strength requirement simultaneously, because volume is low, also can reduce the consumption of obturator cement.

Description

A kind ofly improve additive of filling in mine slip degree of mobilization and preparation method thereof
Technical field
The present invention relates to a kind of new additive agent in filling in mine material, being specifically related to a kind of additive for improving filling in mine slip degree of mobilization.
Background technology
Cut-and-fill Mining Technology is applied more and more wider in mining, in actual stowing operation, filling slurry under certain pump pressure by Cemented filling to dead zone, due to the bleeding of filling slurry, often easily block pumping line.Improve the transportation performance (improving the degree of mobilization of slip) of filling slurry, seem very important.General casting resin slurry main component is tailings or barren rock, cement, water, for improving its mobility, often needs the amount regulating cement and the water added.But in application process, the impact of volume size on Strength of backfill and mobility of cement and water is conflicting.
Intensity and mobility requirement to be met simultaneously, suitable additive must be added.Because filling slurry exists the features such as volume is large, concentration is low, cement mixing content is low.For these characteristics of obturator, it is large to there is volume in existing additive, and cost is high, although its mobility can be improved, and the shortcomings such as filling slurry early strength is undesirable.
Summary of the invention
The object of this invention is to provide a kind of for filling in mine slip, the additive that can meet mobility and early strength requirement simultaneously.
The additive of raising filling in mine slip degree of mobilization provided by the invention, be prepared from by following raw materials according by weight percentage: beta-naphthalenesulfonic-acid salt formaldehyde condensation products 35% ~ 45%, polyvinyl alcohol 2% ~ 5%, calglucon 4% ~ 10%, Tai-Ace S 150 1% ~ 2%, citric acid 15% ~ 18%, water 20% ~ 42%, adds up to 100%.
The preparation method of above-mentioned additive, comprises the steps:
(1) according to described weight percent, water is added reactor, then add beta-naphthalenesulfonic-acid salt formaldehyde condensation products, polyvinyl alcohol and calglucon, stirring reaction;
(2) slowly Tai-Ace S 150 is added, stirring and dissolving, reaction;
(3) add citric acid to react, the obtained described additive of cooling; The reaction of described step (1), (2) and (3) keeps temperature to be 80 DEG C ~ 85 DEG C.
Step (1) stirring reaction preferably 20 ~ 40 minutes.Step (2) stirring and dissolving, reaction preferably 0.8 ~ 1.2 hour.Step (3) reaction preferably 3 ~ 5 hours.
Above-mentioned additive is improving the application in filling in mine slip degree of mobilization, add that quality is cement consumption 0.2% ~ 0.5% of additive.
Beta-naphthalenesulfonic-acid salt formaldehyde condensation products is a kind of aniorfic surfactant, join after in tailings grout, cement particle surface can be adsorbed on, formation hydrophobic group is inside, and one deck adsorption layer that hydrophilic group is outside, because hydrophilic group is electronegative, be equivalent to the electric charge that in slurry, each cement particle surface band is identical, because same sex electric charge repels mutually, unsteady paste structure is originally disintegrated, discharge the free water of parcel, thus increase considerably its mobility.Polyvinyl alcohol makes filling slurry not produce sedimentation and excreting water phenomenon by bridging effect.By above effect, effectively can improve the transportation performance of filling slurry, improve the degree of mobilization of slip.
Additive of the present invention is brown liquid, adds when configuring filling slurry, add that quality is cement consumption 0.2% ~ 0.5%.Concrete volume determines according to the increased value of filling slurry mobility and strength of filling mass.After using additive of the present invention, can pulp density be improved, reduce cement-sand ratio simultaneously, improve the early strength of obturator, enable filling slurry reach requirement of strength fast.In addition, additive of the present invention is low due to volume, also can reduce the consumption of obturator cement.It is estimated, slip per ton can reduce cement consumption 60kg, economic benefits.
Embodiment
The present invention's beta-naphthalenesulfonic-acid used salt formaldehyde condensation products (solid-state) is commercially available, and preferable weight-average molecular weight is 5000 ~ 20000; Being not particularly limited the kind of described salt, such as, can be sodium salt.The molecular weight of the present invention to polyvinyl alcohol does not have particular requirement, and the scope of general molecular weight can be: 110000 ~ 130000.Below by way of specific embodiment, the present invention will be described in detail.
Embodiment one
Prepare raw material by weight percentage: beta-naphthalenesulfonic-acid salt formaldehyde condensation products 35%, polyvinyl alcohol 2%, calglucon 5%, Tai-Ace S 150 1%, citric acid 15%, water 42%; First water is added reactor, again beta-naphthalenesulfonic-acid salt formaldehyde condensation products, polyvinyl alcohol, calglucon are added, keep temperature 80 DEG C always, stirring reaction 30 minutes, slowly add Tai-Ace S 150 stirring and dissolving, reaction after 1 hour, adding citric acid reacts 3 hours again, and cooling obtains additive of the present invention.
Adopt following method to test the performance of additive prepared by the present embodiment, the results are shown in Table 1, table 2.
degree of mobilization is tested: measure its degree of mobilization with instrument for testing fluidity of colloidal cement sand (model NLD-3), measuring method is as follows:
1) divide two-layer loading die trial by the glue sand sample mixed, the first layer height is 2/3, with pocket knife in each stroke of both direction 5 times, draws evenly smash pressure for 10 times 10 times with pocket knife, completely strikes off die trial; .
2) die trial is vertically mentioned gently, start jumping table, complete 30 times in 30 ± 1s and beat;
3) beat complete, with the diameter in kind of calliper glue sand basal diameter and perpendicular direction, calculating mean value is the degree of mobilization of this sample, and this test must complete in 5min.Measurement result is in table 1.
2. intensity test:
Adopt tailings, PC32.5 cement, coordinate by the cement-sand ratio of table 2.Additive prepared by the embodiment 1 of mixing different amount by table 2 mass ratio in slip.Stir evenly and they be cast in 7.07cm × 7.07cm × 7.07cm tri-joint-trial mould, ensureing that in test block casting process, slip does not precipitate, adopting that limit is stirred, marginal not mould build mode.Finally by pressing machine 3 days, 7 days, the 28 days intensity that records test block, obtain uniaxial compressive strength in table 2.
Table 1 degree of mobilization test result
Table 2 strength of filling mass test result
As seen from table, after adding this product, its mobility can be increased substantially, and obturator early strength can be improved.As a comparison, the present inventor be investigated additive be beta-naphthalenesulfonic-acid salt formaldehyde condensation products and polyvinyl alcohol two kinds of materials mixing (quality proportioning 35:2) time obturator degree of mobilization and intensity.The results are shown in Table 3, table 4.
Table 3 degree of mobilization test result
Table 4 strength of filling mass test result
Contrasted from table 1 ~ 4: additive be beta-naphthalenesulfonic-acid salt formaldehyde condensation products and polyvinyl alcohol two kinds of materials time, though obturator degree of mobilization can be improved, obturator early strength can not be improved.The present invention can reach the ideal effect not only improving degree of mobilization but also improve early strength.
Embodiment two
By weight preparing raw material by weight percentage: beta-naphthalenesulfonic-acid salt formaldehyde condensation products 45%, polyvinyl alcohol 5%, calglucon 10%, Tai-Ace S 150 2%, citric acid 18%, water 20%; First water is added reactor, again beta-naphthalenesulfonic-acid salt formaldehyde condensation products, polyvinyl alcohol, calglucon are added, keep temperature 85 DEG C always, stirring reaction 30 minutes, slowly add Tai-Ace S 150 stirring and dissolving, reaction after 1 hour, adding citric acid reacts 5 hours again, and cooling obtains additive of the present invention.
Test the performance of additive prepared by the present embodiment by the method for embodiment 1, test result is in table 5 and table 6.
Table 5
Table 6

Claims (7)

1. one kind is improved the additive of filling in mine slip degree of mobilization, it is characterized in that being prepared from by following raw materials according by weight percentage: beta-naphthalenesulfonic-acid salt formaldehyde condensation products 35% ~ 45%, polyvinyl alcohol 2% ~ 5%, calglucon 4% ~ 10%, Tai-Ace S 150 1% ~ 2%, citric acid 15% ~ 18%, water 20% ~ 42%, adds up to 100%; It is prepared from by following step:
(1) according to described weight percent, water is added reactor, then add beta-naphthalenesulfonic-acid salt formaldehyde condensation products, polyvinyl alcohol and calglucon, stirring reaction;
(2) slowly Tai-Ace S 150 is added, stirring and dissolving, reaction;
(3) add citric acid to react, the obtained described additive of cooling;
The reaction of described step (1), (2) and (3) keeps temperature to be 80 DEG C ~ 85 DEG C.
2. additive according to claim 1, is characterized in that the weight-average molecular weight of beta-naphthalenesulfonic-acid salt formaldehyde condensation products is 5000 ~ 20000.
3. a preparation method for additive described in claim 1 or 2, comprises the steps:
(1) according to described weight percent, water is added reactor, then add beta-naphthalenesulfonic-acid salt formaldehyde condensation products, polyvinyl alcohol and calglucon, stirring reaction;
(2) slowly Tai-Ace S 150 is added, stirring and dissolving, reaction;
(3) add citric acid to react, the obtained described additive of cooling;
The reaction of described step (1), (2) and (3) keeps temperature to be 80 DEG C ~ 85 DEG C.
4. preparation method according to claim 3, is characterized in that step (1) stirring reaction 20 ~ 40 minutes.
5. the preparation method according to claim 3 or 4, is characterized in that step (2) stirring and dissolving, reaction 0.8 ~ 1.2 hour.
6. preparation method according to claim 5, is characterized in that step (3) reaction 3 ~ 5 hours.
7. additive described in claim 1 or 2 is improving the application in filling in mine slip degree of mobilization, add that quality is cement consumption 0.2% ~ 0.5% of additive.
CN201410275390.3A 2014-06-19 2014-06-19 A kind ofly improve additive of filling in mine slip degree of mobilization and preparation method thereof Expired - Fee Related CN104016613B (en)

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CN109987869A (en) * 2019-03-13 2019-07-09 金泰成环境资源股份有限公司 A kind of New Mine filling enhanced additive of rapid hardening

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1270150A (en) * 1999-04-14 2000-10-18 济南华迪有限责任公司 Composite additive for concrete
CN1559964A (en) * 2004-02-26 2005-01-05 同济大学 High performance concrete pumping agent controlling falling degree loss type
JP4206032B2 (en) * 2003-11-21 2009-01-07 日本植生株式会社 Mortar material or concrete material spraying method
CN102923991A (en) * 2012-10-23 2013-02-13 王建东 Concrete multifunctional corrosion remover and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1270150A (en) * 1999-04-14 2000-10-18 济南华迪有限责任公司 Composite additive for concrete
JP4206032B2 (en) * 2003-11-21 2009-01-07 日本植生株式会社 Mortar material or concrete material spraying method
CN1559964A (en) * 2004-02-26 2005-01-05 同济大学 High performance concrete pumping agent controlling falling degree loss type
CN102923991A (en) * 2012-10-23 2013-02-13 王建东 Concrete multifunctional corrosion remover and preparation method thereof

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