JPS63210048A - Hydraulic fine powder material and manufacture - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a hydraulic fine powder material and a method for producing the same.

Conventional technology In the conventional cement industry, the mainstream of grinding cement, which is a hydraulic material, is a closed-circuit method using a ball mill, and the fineness of practical cement is 3,000 to 3,000 in Blaine specific surface area.
4,000al19 (maximum particle size 100-60μm)
It is. Grind cement into highly fine powder! As a method, there is a method using a grinding aid, but even if this method is used, the Blaine specific surface area is about 6,000 d/9, and its use is limited due to the high cost and its characteristics. The reasons for this are that the particle size of the product varies over a wide range, and that the thermal energy of crushing causes morphological changes in the gypsum, which adversely affects quality. In addition, attempts have been made to pulverize slag powder used in blast furnace cement using a vertical roller mill, but as the material to be pulverized becomes pulverized, it becomes difficult to get caught in the gap between the roller and the table. Due to the occurrence of short Ifs in the circulating material, the fineness is at most 6.0% in terms of Blaine specific surface area, similar to ball mills.
000 cJ/p. Closed-circuit grinding systems using ball mills and vertical roller mills are both equipped with separators within the system (1), and the entire system is called the grinding process, but for hydraulic materials such as cement, Blaine specific surface area A closed-circuit pulverization system that can actively control the maximum particle size and particle size range of fine powder of 6.000 d79 or more has not yet appeared.

The present inventors have already ground the hydraulic raw material described in Claim 111 (hereinafter referred to as hydraulic raw material) in a ball mill to a Blaine specific surface area of 3,000 to 6,000c4/9, and then used an air classifier to It was confirmed that by classifying at a classification point of approximately 10 μm, an excellent hydraulic fine powder material having a particle size of 15 μm or less and containing 90% by weight of grains could be obtained.

The hydraulic fine powder material obtained by this method has high hydraulic properties and takes advantage of the well-regulated particle size distribution.
It has been found that it is extremely effective as a main component of mortar, concrete, and grout materials that have a variety of properties. Based on these findings, the present inventors have developed a hydraulic fine powder material obtained by this manufacturing method.
Grout material with injection hardening properties in 5 years [Product name 8 Iron Super Fine] and fine slag powder based cement reinforcement material [Product name: 8 Iron Super Fine]
Developed products such as "Nippon Steel Spirits".

Problems to be Solved by the Invention However, since this manufacturing method includes two steps: a pulverization step using a ball mill and a classification step using an air classifier, the throughput of the classification step is small and the mass balance does not match. Equipment costs are high because transportation and storage equipment is required, the yield is low because the hydraulic material before classification contains a large amount of coarse powder, and equipment is also required to process the coarse powder after classification. Moreover, there is a drawback that the power consumption rate of the manufacturing process is also high. In addition, although there is no problem in single classification of homogeneous hydraulic raw materials such as glassy blast furnace slag (hereinafter referred to as slag), there is no problem in classifying homogeneous hydraulic raw materials such as glassy blast furnace slag (hereinafter referred to as slag). Since there are differences in the pulverizability of the constituent compounds and hydraulic raw materials, the composition of the hydraulic material obtained by crushing with a ball mill and the hydraulic fine powder material after classification are different. Therefore, it is difficult to mix and manage hydraulic raw materials to obtain the desired hydraulic fine powder material.

Means to Solve the Problems In view of the above-mentioned circumstances, the present inventors have conducted repeated pulverization experiments with the aim of obtaining the required hydraulic fine powder material using only a direct pulverization process, which is not available in conventional manufacturing methods. As a result, we were able to achieve this objective by using a closed circuit pulverization method using a dry media stirring mill.

That is, the present invention provides a manufacturing method C comprising two steps: a pulverization step using a ball mill and a classification step using air current classification [K].
Hydraulic fine powder material of the same quality as the hydraulic fine powder material manufactured by the conventional manufacturing method) is finely pulverized using a closed circuit pulverization method using a dry media stirring mill, which is completely different from the conventional manufacturing method. This is a manufacturing method obtained by

The characteristics of the dry media agitation mill are as follows: (1) Since the grinding action is based only on the grinding action using a high grinding media pressure, continuous grinding is possible without the cushioning action that occurs in ball mills. ■
Since the grinding media filled in the mill body is simply stirred by the stirring shaft, the grinding power is low. ■Since the grinding action is based only on the grinding action, the rise in the grinding temperature is small. ■ Particle size can be easily adjusted by adjusting the feed rate of raw materials and the air flow rate inside the mill body.

The method of the present invention is shown below.

Hydraulic raw materials stored in a storage hopper or the like are drawn out by an extractor and fed to a dry media stirred mill. At this time, grinding aids (diethylene glycol,
Triethanolamine, etc.) is preferably added to the stone. The supplied hydraulic raw materials are finely pulverized by a grinding action in a dry media agitation mill, and then classified by a separator in the system. It is discharged from the system and stored in a storage silo as hydraulic fine powder material.

On the other hand, the coarse powder classified by the separator is returned to the dry media stirring mill and re-pulverized. As described above, the manufacturing method of the present invention is characterized in that fine pulverization is carried out using the dry medium stirring mill 1 (closed circuit pulverization method).

Example The following will be explained based on examples.

Each hydraulic raw material used in Example 1.2.3.4 is from the same rod, and each chemical composition is as shown in Table 3.

Table 1 Chemical composition of hydraulic raw materials used Example 1 A tower mill, which is a type of dry media stirring mill, was prepared by adding 0.1 weight of a grinding aid (diethylene glycol) to dried slag based on the amount of slag supplied. (KD-100 model manufactured by Nippon Tower Mill ■) and passed through a separator to obtain a fine slag powder of the present invention.

On the other hand, for comparison, using the same slag in a cement ball mill, the Blaine specific surface area was 4.200 by adding 0.1 weight of duckweed to the amount of ll auxiliary agent (diethylene glycol) slag supplied.
J/PK pulverization was performed using an air classifier to obtain a slag fine powder for comparison at a classification point of approximately 109 m. The particle sizes of the fine slag powder of the present invention, the comparative fine slag powder, and the general-purpose slag powder of Blaine specific surface #i44,200t) were determined by laser diffraction method [■Seishin Enterprise SK LASER
FIG. 1 shows the results measured using MICRON 5IZBR. The particle size of the fine slag powder of the present invention and the fine slag powder for comparison were almost the same, and the content of particles of 15 μm or less was 97% by weight or more.

In order to explore the effect of the fine slag powder of the present invention as a cement admixture, Blaine specific surface i3.1201'2
50 of Ordinary Portland Cement (hereinafter referred to as OP)
The material (hereinafter referred to as N
Using a material (hereinafter referred to as NS) in which 50% by weight of OP was replaced with comparative fine slag powder (hereinafter referred to as T) and a material in which 50% by weight of OP was replaced with general-purpose slag powder (hereinafter referred to as NB). A mortar strength test was conducted based on JISR5201.

The results are shown in Table 2.

From Table 2, it is confirmed that the compressive strength of NT mortar and NS mortar is about 1 times the compressive strength of N8 mortar and 02 mortar at 3 days old, and about 1.4 to 1.5 times stronger at 28 days old. It was done. Furthermore, the strength of NT mortar at 3 and 7 days of age is higher than that of NS mortar. This is thought to be due to the mechanochemical effect that improves the surface activity due to the pulverization caused by the attrition action alone. It was found that the powder and the same material E were of high quality.

Note that the power consumption rate of the manufacturing process of the slag fine powder manufactured by the manufacturing method of the present invention is approximately 30% higher than that of the manufacturing process of the comparison slag fine powder manufactured by the conventional manufacturing method. %, and it was confirmed that the effect of the present invention is remarkable.

Example 2 Portland cement clinker, slag, and gypsum pulverized to a maximum particle size of 5 Ifi+ or less in a mill
Supplied to the clay mill used in Example 1 with the formulation shown in the table,
Add grinding aid (diethylene glycol) to the supplied amount.
, 1iii% of the hydraulic fine powder material T of the present invention, which is finely pulverized and has a particle size of 15 μm or less and contains 95% by weight or more.
-1, T-2, T-3, T-4 (hereinafter T-1, T-2,
(denoted as T-3 and T-4) were obtained.

For comparison, Portland cement clinker, slag, and gypsum were finely pulverized in a cement ball mill with the composition shown in Table 3 1c, and a grinding aid (diethylene glycol) was added to the feed amount by 0.1% by weight. Hydraulic fine powder material B for comparison with a specific surface area of about 6.00Oct/F
-1, B-2, B-3゛, B-4 (hereinafter B-1, B-2
, B-3, and B-4) were obtained.

Table 3: Composition and particle size of hydraulic fine powder material, B-1
Table 3 also shows the grinding power consumption index, where the grinding power consumption of the material is taken as 100%.

Using the hydraulic fine powder material in Table 3, JIS R520
A mortar strength test was conducted based on 1.

The results are shown in Table 4.

Table 4: Mortar strength test At present, ultra-early strength Portland cement with a Blaine specific surface area of 6.000 aA/f and a 1-day compressive strength of about 220 KP/A is suitable for shortening construction periods and temporary repair work. However, ball mills for cement have many problems, such as inefficiency and high cost as they are finely pulverized to a Blaine specific surface area that is close to the limit.

However, according to the manufacturing method of the present invention, the slag composition is 3.
It was confirmed that a hydraulic fine powder material with sufficiently high initial strength even at 0% can be obtained at low cost.

According to the above examples, in the production method of the present invention, it is possible to mix and finely pulverize several types of hydraulic raw materials,
It was found that the obtained hydraulic fine powder material exhibited high hydraulic properties. Furthermore, it was found that a hydraulic fine powder material of the required quality can also be obtained by mixing the fine slag powder of the present invention obtained in Example 1 and T-1 of the present invention obtained in Example 2. Ta.

Example 3 Hydraulic raw materials containing 43% by weight of Portland cement clinker, 53% by weight of slag, and 4% by weight of gypsum, which were ground to a maximum particle size of 5 cm or less in a 0.0 mm mill, were added to the tower mill used in Example 1. Grinding aid (
A hydraulic fine powder material (hereinafter referred to as TS-1) of the present invention containing 100% by weight and a particle size of 15 μm or less was obtained by adding 0.1% by weight of diethylene glycol). For comparison, hydraulic raw materials with the same formulation as in the production method of the present invention,
Hydraulic fine powder material (hereinafter referred to as B5-1) obtained by finely pulverizing the supply amount 1 (to which 0.1% by weight of a grinding aid (diethylene glycol) with a practical ball mill to a Blaine specific surface area of 5,820 cd/9) B5-1 was further classified using an air classifier at a classification point of approximately 10 μm to obtain a hydraulic fine powder material for comparison (hereinafter referred to as B5-2).

The particle size distribution of the present invention and the comparative hydraulic fine powder material are shown in FIG. In order to compare the injection characteristics of each hydraulic fine powder material obtained in this example, the diameter was 551+III+ and the length was 300mm.
Injected sand 11 height + 00 cm at the bottom of the transparent acrylic resin tube of m! (fiura standard sand 0.1 question ~ 0.3 tram,
A porosity of 42% was created, and the injected milk was allowed to flow down by gravity from the funnel on the hill, and the length (penetration length) that the injected milk permeated into the injected sand layer was measured. The results are shown in Table 5.

Table 5: Injection test results From Table 5, the comparative amount (BS-2
), and it was confirmed that infiltration into fine sandy ground is possible.

A similar injection test was also conducted on the fine slag powder of the present invention obtained in Example 1, and the result was that the penetration length was 100 m, and the aggregation rate was slow due to its water use activity.
It was found to have excellent injection properties. In addition, from this example, the power consumption rate of the manufacturing process of TS-1 obtained by the present invention is reduced by approximately 15% compared to the power consumption rate of the manufacturing process of comparative quantity B5-2, which shows the effect of the present invention. was confirmed.

Example 4 Conventionally, the MS method is known as a water glass grout in which slag powder can adjust the gel time and does not reduce strength, but due to the different particle sizes, there are restrictions on the ground to be poured, and the water injection phase ratio has to be set to 1. If an attempt is made to improve the injectability, material separation will occur, which will further result in a decrease in strength. Therefore, in this example, in order to investigate the effect of adjusting the gel time of the fine slag powder of the present invention obtained in Example 1, a part of the TS-1 of the present invention obtained in Example 3 was treated with fine slag powder. Substituted hydraulic fine powder material 08-1.08-2, G5-3.08
-4 (hereinafter 08-1, G5-2.08-3, G5-4
), the experiments shown in Table 6 were conducted.

As shown in Table 6, the fine slag powder of the present invention was found to be able to control gel time and maintain high strength despite its high degree of fineness.

Further, the same experiment was conducted on the comparative fine slag powder obtained in Example 1, and it was confirmed that the powder had properties equivalent to those of the product of the present invention.

It is known that grout material containing Portland cement clinker reacts rapidly when it encounters water containing electrolyte, causing a coagulation and precipitation phenomenon. This can be seen from the fact that when the injected sand layer of 1 is filled with seawater and then the milk of TS-1, the product of the present invention obtained in Example 3, is injected under the same conditions as in Table 5, a penetration length of only 15 steps is obtained.However, , the slag fine powder material of the present invention obtained in Example 1 was found to be 100% in the same injection test.
Fin penetration length was obtained.

Therefore, the fine slag powder of the present invention obtained in Example 1 is useful as a grouting material for mausoleums filled with seawater and hot spring water containing electrolytes. It was found that it is more preferable to add gypsum.

In this example, it was found that the fine slag powder of the present invention obtained in Example 1 has excellent characteristics that greatly expand the range of application of conventional grout materials.

Effect of the invention According to the present invention, there are the following effects.

■Compared to fine slag powder obtained by conventional manufacturing methods, the fine slag powder obtained by the present invention has high hydration hardening properties equivalent to or higher than that of fine slag powder obtained by conventional manufacturing methods. It has certain characteristics.

■According to the present invention, it is possible not only to finely grind slag alone, but also to mix and finely grind materials containing several types of hydraulic raw materials, and the obtained hydraulic fine powder material has excellent early water availability. ,
Has injectability.

In addition, according to the manufacturing method of the present invention, since it is possible to obtain duck as a hydraulic fine powder material, the power consumption rate of the manufacturing process is lower than that of slag compared to the conventional manufacturing method. In the case of fine powder, it is reduced by about 30%, and in the case of hydraulic fine powder material made of several types of hydraulic raw materials, it is reduced by about 15%, which has a cost reduction effect.

■Since the grinding process involves only grinding, the grinding temperature is low, so there is no change in the form of the gypsum.

■Since the composition of the hydraulic raw material in the pulverization section and the hydraulic fine powder material after pulverization are the same, it is easy to mix the hydraulic raw material.

■The particle size range of the required hydraulic fine powder material can be easily adjusted by controlling the feed rate of raw materials and the air flow rate inside the mill.

[Brief explanation of the drawing]

Figure 1 shows the particle size distribution of general-purpose slag powder A obtained in Example 1, comparative fine slag powder B, and fine slag powder C of the present invention, and Figure 2 shows the comparative hydraulic fine powder obtained in Example 3. Powder material (BS-1) D and comparative hydraulic fine powder material (BS-
2)-B, and the hydraulic fine powder material of the present invention (TS-1
) is an explanatory diagram showing the particle size distribution of F.

Claims (3)

[Claims] (1) Fine powder obtained by pulverizing vitreous blast furnace slag, cement clinker, and gypsum alone or a mixture thereof, with a particle size of 15 μm or less and 90% by weight.
Hydraulic fine powder material containing the above. (2) A composition for high strength and high durability mortar/concrete characterized by using the above-mentioned hydraulic fine powder material,
A method for producing ultra-early strength cement and grout. (3) A method for producing a hydraulic fine powder material, which comprises directly pulverizing the hydraulic raw material according to claim (1) using a pulverizer in a closed circuit system.