CN105084804B - Air entraining agent used for reducing entrapped air on surface of filling body and preparation method and application of air entraining agent - Google Patents
Air entraining agent used for reducing entrapped air on surface of filling body and preparation method and application of air entraining agent Download PDFInfo
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- CN105084804B CN105084804B CN201510461460.9A CN201510461460A CN105084804B CN 105084804 B CN105084804 B CN 105084804B CN 201510461460 A CN201510461460 A CN 201510461460A CN 105084804 B CN105084804 B CN 105084804B
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- entraining agent
- air entraining
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- obturator
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Abstract
The invention relates to an air entraining agent used for reducing entrapped air on the surface of a filling body and a preparation method and application of the air entraining agent. The preparation method includes the steps of taking lignin sulfonate, adding water and sodium hydroxide to regulate the pH value to 9-10, conducting heating till the temperature is 60-70 DEG C, adding alkyl benzene sulfonate, conducting heating till the temperature is 80-85 DEG C, conducting heat preservation for a certain period of time, adding incense powder, conducting heating till the temperature is 120-150 DEG C under the production of non-oxidation gas so that the incense powder can be melted, adding formaldehyde during stirring, conducting a heat preservation reaction, conducting cooling till the temperature is 85-90 DEG C, adding carboxymethylcellulose to have a condensation reaction with formaldehyde, stirring a product, and conducting cooling to obtain the air entraining agent. Entrapped air on the surface of the filling body can be reduced by adding the air entraining agent in the stirring, preparing and conveying processes of the filling body; the mobility of the filling body can be improved, and the slump loss can be reduced; the water secreting amount and the porosity are decreased, and the compactness of the filling body is improved; the surface defects of the filling body are reduced, the interface characteristics are improved, and the anti-fracture strength and the compressive strength of the filling body are improved.
Description
Technical field
The present invention relates to it is a kind of for during mining with stowing, for reducing the air entraining agent and its system of obturator surface blister
Preparation Method.
Background technology
Mine tailing cemented filling, is mainly filled using ore dressing plant tailings and cement.Flotation is by adding
Infusion, makes mineral grain float on liquid level to reclaim mineralogical composition with foam as carrier, still there is a certain amount of in tailings
Infusion.In stirring, preparation and course of conveying in casting resin, its foaming agent continues generation effect, and filling slurry is entered after stope,
Cement granules and mineral and mud constitute again foam suspension on obturator surface.
The blister thing constituted again in stowing operation, is the difficult problem of long-standing problem filling technique personnel.It is made in obturator
Cement content is reduced, and causes strength of filling mass to reduce, and wastes cement, increases filling cost, additionally, due to cement mineralses and mud
There is considerable time in form, prevent obturator from solidifying, and affect the enforcement of the method for mining by the way of filling.
The content of the invention
For the drawbacks described above of prior art, it is an object of the invention to provide a kind of air entraining agent and preparation method thereof, energy
Enough reduce obturator surface blister and improve filling bulk properties.
The preparation method of the air entraining agent of the reduction obturator surface blister that the present invention is provided, comprises the following steps：
（1）80～100 parts of lignosulfonate is taken by mass parts, adds water and sodium hydroxide to adjust pH value to 9～10, heated
To 60 ~ 70 DEG C；
（2）10～20 parts of alkylbenzenesulfonate is added, 80 ~ 85 DEG C is heated to, insulation a period of time；
（3）10～30 parts of Colophonium powder is added, under non-oxidizing gas protection 120～150 DEG C are heated to, melt Colophonium powder
Melt, stirring is lower to add 5～18 parts of formaldehyde, insulation reaction；
（4）85 ~ 90 DEG C are cooled to, add 0.8～1.8 part of carboxymethyl cellulose to carry out condensation reaction with above-mentioned formaldehyde, produced
Obtain final product after thing stirring, cooling.
The alkylbenzenesulfonate is preferably dodecyl benzene sulfonate.
The lignosulfonate molecular weight is preferably 3500 ~ 6000, and sulfonation degree is preferably 1.1 ~ 1.9mmol.g-1。
Step（2）Insulation is preferably 30 ~ 50 minutes.Step（3）Insulation reaction is preferably 30 ~ 50 minutes.Step（4）Condensation
Reaction is preferably 50 ~ 80 minutes.Step（4）Product stirring is preferably 20 ~ 40 minutes.
Application of the air entraining agent of above-mentioned reduction obturator surface blister in filling in mine, by cement weight 0.01%～
0.1% is added to air entraining agent in filling slurry.
The above-mentioned obturator air entraining agent of very low amounts is mixed in obturator stirring, preparation and course of conveying, makes filling internal
Portion produces and is uniformly distributed micro-bubble that is stable and closing in a large number, and it is distributed in obturator structure, has both enclosed obturator knot
Many capillary channels in structure, can form hydrophobic film in hydrated cementitious mineral surfaces again reduces capillary tube swabbing effect, it is suppressed that fill
Body stirring is filled out, prepared, conveyed flotation effect of the disturbance to cement.The disturbed movable property of bubble in obturator stirring, preparation, course of conveying
Raw migration, minute bubbles and into air pocket gradually rise to obturator surface and vanish.So, in obturator stirring, prepare, convey
During add the present invention air entraining agent can reduce obturator surface blister.
The air entraining agent of the present invention has the following advantages：Adding in obturator stirring, preparation, course of conveying can reduce obturator
Surface blister；Filling liquid flowability can be improved, slump-loss is reduced, and has certain water-reduction；Reduce bleeding quantity and hole
Gap rate, improves the degree of compaction of obturator；Obturator surface defect is reduced, improves interfacial characteristics, improve obturator anti-folding and anti-pressing strong
Degree, or reduce cement consumption.
Specific embodiment
Lignosulfonate used of the invention, is the side-product of sulphite process papermaking wood pulp, can be purchased from market.It is
Through the lignin of sulfonation modifying, as long as being connected to sulfonic group on the side chain or phenyl ring of lignin molecule, molecular weight is excellent
Elect 3500 ~ 6000 as, sulfonation degree is preferably 1.1 ~ 1.9mmol.g-1.Alkylbenzenesulfonate used of the invention, for example, can be ten
Dialkyl benzene sulfonate.
The obturator air entraining agent of embodiment 1-6 is prepared into by the proportioning feeding of table 1, is prepared using following methods：
（1）Take lignosulfonate（It is purchased from distance of travel of roc chemical products company limited, brown powder thing, pH value 7 ± 1, moisture≤
7%, calcium-magnesium content≤1.5%）In reactor, add water and sodium hydroxide to adjust pH value to 9～10,65 are heated to while stirring
℃；
（2）Again plus dodecyl benzene sulfonate is in reactor, 85 DEG C are heated to, 40 minutes are incubated；
（3）Colophonium powder is added, 120～150 DEG C are heated under nitrogen protection, melt Colophonium powder, what is be stirred continuously
In the case of add formaldehyde, insulation reaction 40 minutes；
（4）When being cooled to 90 DEG C, carboxymethyl cellulose is added to carry out condensation reaction 1 hour with formaldehyde；
（5）Product is quickly stirred 30 minutes after above-mentioned reaction, and the product that solution shape is obtained after cooling is present invention filling
Body air entraining agent.
Table 1
Obturator air entraining agent of the present invention is mainly used in filling in mine, for obturator air entraining agent prepared by embodiment 1-6
Application effect test：
（1）Prepare a kind of slurry samples of inspection obturator air entraining agent effect：From certain gold ore tailing, normal silicate water
Mud, by cement：Tailings is 1:6 cement-sand ratio, mass concentration 68% prepares filling slurry sample；
（2）Obturator air entraining agent of the present invention is added in filling slurry by the 0.01%～0.1% of cement consumption, is stirred
Mix, prepare, convey；
（3）The assay method of the filling slurry slump is：Filling slurry mixture is loaded in slump cone（Slump cone
Inside dimensions are：Top diameter 10cm；Base diameter 20cm；Height 30cm）, unnecessary slip and floating with spatula is scraped off, it is double
Handss uniformly firmly lift in cylinder.Filling slurry will produce slump phenomenon due to deadweight, by slump cone top to the slip for collapsing
The distance at top（Unit：Cm or mm）Just the slump is, as the liquidity scale.The bigger mobility for representing mixture of the slump
It is bigger, but while also want the situation of the cohesiveness of comprehensive observing slip, water-retaining property.
The filling slurry of addition obturator air entraining agent of the present invention is by stirring, preparing, being delivered to the bubble that goaf produces
It is little and uniform, compare the bubble produced without obturator air entraining agent and reduce about 90%, when addition is 0.08%, obturator contains
Tolerance is 7%, improves dispersive property, and cement is fully contacted with water, enables cement to obtain sufficient hydration reaction.Meanwhile, addition
The filling slurry of obturator air entraining agent of the present invention can significantly improve comprcssive strength（It is shown in Table 2）；Mobility is improved, slump is reduced and is damaged
Lose（It is shown in Table 3）.
Table 2
Table 3
Obturator air entraining agent raw material of the present invention is easy to get, and simple production process is easy to operate, can be widely used in mine and fill
Fill out；Bleed effect preferably, can comprehensively improve the performance of obturator, when tret is in 0.01～0.08%, air content≤7%, filling
3 days, 7 days and 28 days bending and compressive strengths of body can improve 5%～30%；When tret is 0.01～0.08%, reduces filling slurry and collapse
Degree of falling loses 0.2～1 ㎝；There is more hydrophilic group, there is stronger affinity to free water, reduce the bleeding of obturator
Rate, reduces the space of obturator, increased the degree of compaction of obturator.
Claims (6)
1. a kind of preparation method of the air entraining agent for reducing obturator surface blister, it is characterised in that comprise the following steps：
（1）80～100 parts of lignosulfonate is taken by mass parts, adds water and sodium hydroxide to adjust pH value to 9～10, be heated to 60
~70℃；
（2）10～20 parts of alkylbenzenesulfonate is added, 80 ~ 85 DEG C are heated to, 30 ~ 50 minutes are incubated；
（3）10～30 parts of Colophonium powder is added, under non-oxidizing gas protection 120～150 DEG C is heated to, melt Colophonium powder,
Stirring is lower to add 5～18 parts of formaldehyde, insulation reaction 30 ~ 50 minutes；
（4）85 ~ 90 DEG C are cooled to, add 0.8～1.8 part of carboxymethyl cellulose to carry out 50 ~ 80 points of condensation reaction with above-mentioned formaldehyde
Clock, obtains final product after product stirring, cooling.
2. the preparation method of the air entraining agent for reducing obturator surface blister according to claim 1, it is characterised in that described
Alkylbenzenesulfonate is dodecyl benzene sulfonate.
3. the preparation method of the air entraining agent for reducing obturator surface blister according to claim 1, it is characterised in that described
Lignosulfonate molecular weight is 3500 ~ 6000, and sulfonation degree is 1.1 ~ 1.9mmol.g-1。
4. the preparation method of the air entraining agent for reducing obturator surface blister according to claim 1, it is characterised in that step
（4）Product is stirred 20 ~ 40 minutes.
5. a kind of air entraining agent for reducing obturator surface blister, it is characterised in that prepared by one of claim 1 ~ 4 methods described
Form.
6. application of the air entraining agent of obturator surface blister in filling in mine is reduced described in a kind of claim 5, and its feature exists
In air entraining agent is added in filling slurry by the 0.01%～0.1% of cement weight.
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Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1169404A (en) * | 1996-06-24 | 1998-01-07 | 张显军 | Plasticizing lead gas for building mortar and concrete, lead gas water-reducer and preparation technology thereof |
| CN100400458C (en) * | 2005-01-04 | 2008-07-09 | 华南理工大学 | Lignins metro shield grouting additive and its preparation method |
| CN101328037B (en) * | 2008-07-31 | 2010-12-08 | 华南理工大学 | Alkali lignose concrete air-leading water-reducing agent, preparation and use thereof |
| CN102701633B (en) * | 2012-06-28 | 2014-06-04 | 武汉常阳新力建设工程有限公司 | High-efficiency concrete air entraining agent and preparation method thereof |
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