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Proceedings: Symposium on Evolution of ‘Abandoned Mine Land Technologies Riverton, Wyoming dune 14 16, 1989, Sodium Silicate Grouts: The Solution to Difficult Subsidence Problems Richard H. Reifsnyder- John F. Peters Introduction In 1982, the PQ Corporation was: approached: by the Office’ of Surface Mining, Reclamation ‘and Enforcement and asked to develop a grouting technique that would enhance the placement of cement mixes under water. The standard technique being used in. remedial » actions : to prevent subsidence was to inject a fly ash/cement grout into the void to form high strength columns that would provide support to the collapsing ‘overburden. Once the overburden was stabiized, the void is then filed using a backfill or low strength grout. This technique worked well in dry mines but has not proven effective when water was, Present within the mine void." To form high angle of repose support columns using a fly ash/cement grout, the self-supp properties of the mix is controlled by adjusting the ‘solids content of the grout. The higher the solids of the grout, the lower the slump value and the faster the grout would build a column. The problem encountered in flooded mines was that once the grout was injected into the void the surrounding water would penetrate into the mix diluting the grout and reducing its self-supporting properties.” This dilution caused the grout to level out forming a low angle of repose mass on the void floor. To achieve roof contact and adequate support, large Volumes of grout would have: to::be injected thereby raising the total.cost of the raw: materials, needed to complete a job.” Other problems were encountered when grouting flooded mines. Typical mixes were designed to reduce costs by increasing the ratio of fy ash to. cement used. Mixes based on 6 to 1 fly ash to cement by volume are commonly used to control ‘costs.’ When high compressive strength grouts (@,000 to 5,000 psi) are required, a sand aggregate also included in the mix. These grouts are effective:in dry environments but when injected into water, the fly ash and cement components were found to separate due to their differences in density. This results in a large mass of grout ‘composed mainly of fy ash that does not set up and has no load bearing, capacity to provide support to the overburden.’ Also, in many cases the water in the mine would be flowing, which tended to displace the grout away from the placement site. Moving water can also erode structures builtin the void before the grout can set. ‘These were the major problems the OSMR&E asked PQ to solve. To accomplish this, a laboratory study was conducted to evaluate the behavior of fly ash cement grouts in water on a {Senior Technical Service Reprosantative, PQ Corporation, “*Markot Development Project Managar, PQ Corporation Sodium Silicate Grouts: ‘small scale. Different grout mixes were injected into water and then observed for rate of height development and durabiity of the final structure. Compressive strength was also measured for samples which had set in water. This study revealed that silicate can significantly improve the performance of grouts placed in water.” When ‘mixed into the grout prior to injection, the silicate improved the final strength of the grout and had a positive effect on column formation. It was also found that if silicate was injected into the water prior to or during grout placement there was a significant improvement in column angle of repose and the final structure had improved physical properties. Based on these results, a pilot scale mine simuiation was conducted to evaluate these effects under conditions found in actual mines. The results ofthis study have been published under the title "Sodium Silicate Grout Technology for Effective Stabilization of Abandoned Flooded Mines" and U.S. patent 4,804,297. Chemistry The chemistry that allows this process to work is. based on the reactivity of soluble silicon dioxi with muttivalent cationic metals such as calcium. Historically, soluble silicates have been used as ‘cement modifies to yield mixtures with accelerated set times; increased compressive strengths and improved acid resistance.’ Established end uses where the improved properties imparted by silicates are made use of include water resistant grouting, oil field cementing, hazardous waste solidification and acid resistant cements. In these applications, the silicon dioxide component of the soluble’ silicate reacts with sources of calcium present in the cement (soluble calcium, calcium ‘oxide and calcium hydroxide) to form various calcium silicate compounds that hydrate with water and increase the rate and number of bond sites formed between aggregates.’ When added to a cement sluny, the silicate quickly reacts to produce these bonds and accelerates the setting of the mix. The hydrated calcium silicate compounds produced from this reaction improve the final physical properties of the cement mixture by increasing the number of bonds formed between the cement and aggregate particles.” Calcium silicate is the active component of all Portiand Cement systems and is responsible for the setting ‘and solidfication reactions when water is added. By adding a soluble silicate to the mix and introducing a source of reactive silicon dioxide, a reactive form of Portland cement in situ ‘is produced." Since the silicon dioxide is already in a soluble form, the resultant calcium silicate produced is hydrated more quickly than the anhydrous. calcium slicate contained in the cement." This is why controling the additon level of silicates in modified cement systems allows significant changes in the rate of set. While the addition of sicate into a cement grout does improve its behavior when placed under water, it does not completely eliminate all the problems that prevent effective stabilization of flooded mines. The increased number of bonds between the grout particles does help reduce the separation of fy ash and cement when the grout is injected in water, and the controlled set of the grout helps to eliminate erosion of grout columns. by moving water, but there can be limitations to this approach. The most important of these is the speed of the reaction when cement and silicate are combined before placement. When mixed, the calcium silicate formed immediately stats to bond aggregate particles together."” The initial bonds formed are sensitive to shear and when the ‘modified mix is pumped through the grout lines, the bonds are easily disrupted or broken. Once broken, these bonds are not readliy reformed, 30 there is a reduction in the benefits associated with the addition of siicate.* Laboratory data indicates that the breaking of the initial bonds formed can reduce the final compressive strength of a siicate modified cement by as much as 23%."* ‘An even greater limitation associated with mixing silicate directly into a cement grout is the negative effect. has on the handling and pumping characteristics of the mix. To successfully place the grout into a mine void, the mix must be transferred through lines or hoses trom the mixer to the. void. The lengths of these lines and the distances the grout must travel are large and in some cases can exceed 700 feet." The effect silicate has on grout set times can-cause the mix tolincrease in viscosity rapidly, which increases the resistance the grout has to moving and the pumping pressures required. In many cases, the grout will have the tendency to set up too quickly Which resutts in plugging of the grout lines and causing considerable down time and increased labor to clear the lines. Through extensive testing, it has been demonstrated that_ the self-supporting characteristics of the silicate modified grout and the final angle of repose of the formed columns can be effected by penetration of the surrounding water into the grout matrix after placement. When intially injected into water, a silicate modified grout will form a high angle of repose structure (35° or greater) but with time, water is forced into the grout due to osmotic pressure, which causes the grout mass to swell and disrupts many of the calcium silicate bonds that have been formed." This results in a slumping of the grout and a Sodium Silicate Grouts: - oad ca Sed 80 Inner Pipe = 001225 fe outer Pipe = 2002080 #42 sosulus = oroaost £22 5 Taner Pipe = 1.500 tm, é Queer Pipe => 1,939 ta. ' admutar Gop = 0.0195 ta, nacto 1" Mane coupling —1 1/2" sea 80 sed 60 1" on 2" Saddte (6 @'90* co one another) y Taner/agoular Ares ‘AP 105 pet / gpm ve. 110 pat/spe, ‘calculated NOT TO SCALE eiicate atx out Cross Sectional Ares 15.12 - actual (Faure 1) Annulus Nozzle reduction of the column height and angle of repose. Grout structures formed underwater havebeen found to deteriorate rapidly and lose height and subsequent roof contact in as litle as, fifteen minutes."” To eliminate these problems associated with silicate modified grouts, a grouting technique was developed that would allow for effective placement of these mixes. This technique relies on the use of an annulus nozzle (figure 1) which combines silicate and cement grout at the point of placement instead of in the grout mixer. As the grout stream ‘enters the water at the line exit point, a stream of liquid si rout by the nozzle. This forms a curtain of silicate around the grout which reacts with the grout stream surface before the grout come into contact with the water. This surface reaction promotes the formation of a calcium silicate gel layer that prevents water from Penetrating the mix and reducing its self ‘Supporting properties."” As a result, the grout can form high angle of repose columns which will not degrade over time. Laboratory and field data have demonstrated that this technique is superior to the process of mixing the silicate into the grout mix prior to injection. Data on compressive strength of grouts set this way underwater shows that the silicate enhances the ultimate strength of the set grout while providing the other benefits that contribute to good

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