Laboratory work №2 Theme lessons: Research of the properties of natural siliceous raw materials

The purpose of lessons: the study of the physical and mechanical, chemical and physical properties of natural siliceous materials, evaluation of the suitability of materials for thermal insulation foam glass technology building purpose.

The plan of lessons

1. Introduction to the procedure of GOST 16381 - 77. Building materials and products insulating. Classification and general technical requirements.

2. Introduction to the method of GOST 17177 - 94. Building materials and products insulating. Test methods.

3. Introduction to the method of GOST (STB) 1322 - 2002 blocks of insulating foam glass. Specifications.

4. The study of the physical and mechanical, chemical and physical properties of natural siliceous materials

5. Assessment of the suitability of materials for thermal insulation foam glass technology building purpose

6. Burning opoks and obtain a building foam glass thermal insulation destination

Running time of work – 3 hours

Brief theoretical information

From a physical point of view, foam glass is a heterogeneous system, the gaseous and solid phases, in which the gaseous phase occupies more than 90% of the total. Thus, it is a solidified foam with closed cells of polyhedral forms which by their size, shape and nature of the distributions are very uniform. This cell structure foam glass makes some outstanding properties, especially low water absorption and high mechanical strength at low volume weight.

This type of cellular insulation material has nearly a century of development and its products are widely used in construction throughout the world.

The first foam glass was obtained in the Soviet Union in the thirties of the last century, the famous scientist and expert in glass I.I. Kitaygorodskiy. Then the former Soviet Union were four plant for the production of foam glass. Later this material (for various reasons), "has been forgotten".

Foam glass – a cellular thermal insulating material obtained by sintering a mixture of glass powder and blowing agent from the foam, followed by annealing.

Burning - heating and holding at a high temperature (in kilns) of different materials to impart desired properties or remove impurities.

Opoks - light, dense fine siliceous sedimentary rocks up to 97% consist of the smallest (0,005-0,001 mm) isometric and irregular particles of aqueous amorphous silica.

Blowing agents - agents with which the system then creates a monolithic material.

Thermal insulation properties - the ability of a material to store heat.

Thermal insulation materials - materials that are characterized by low thermal conductivity, are used for thermal insulation of buildings and structures, industrial equipment, pipelines, etc.

Equipment, tools and technical means: natural siliceous raw materials; jaw crusher; metal or porcelain mortar; technical and analytical balances; fireclay or porcelain crucible; muffle furnace.

The order of performance of works in the audience:

1. Master students familiarize with the procedures of GOST 16381 - 77. Building materials and products insulating. Classification and general technical requirements. GOST 17177 - 94. Building materials and products insulating. Test methods. GOST (STB) 1322 - 2002 blocks of insulating foam glass. Specifications.

2. After studying the necessary information master students studying the physic-mechanical and physic-chemical properties of the natural siliceous materials

3. Then master students evaluate raw materials suitable for heat-insulating foam glass technology building purpose

The main raw material used in the production of building heat-insulating foam glass purpose is siliceous sedimentary and biochemical origin - opoks.

Siliceous sedimentary rocks biochemical in Kazakhstan presented opoks, opoka-like sandstones and clays, diatomite, tripolis spongolite. Their mineralogical and chemical characteristics is that they consist of compacted to varying degrees of siliceous residues of diatoms, radiolarians and sponge needles composed of silica.

The silica content in opoks Kazakhstan deposits ranging from 57.7 to 85.97%, diatomite from 62.6 to 83.65%, tripoli from 67.56 to 76.0% and from 91.3 spongolite to 93.6%.

On the territory of Western Kazakhstan is widely known deposits of diatomite, tripoli, and opoks that are suitable for the production of thermal insulation products (Utesay, Kyrgyz, Shipovsk, Kok Norinsk, Akbulak, Ispai-Bulak, Aksu). Other deposits (Kuduk, Izembet, Derkul) still poorly understood and further work is required to determine the quality of raw materials and its suitability in various industries.

In Northern Kazakhstan is known a large number of deposits and occurrences of opoks and tripoli, suitable for the production of expanded clay (Kachar, Novoiliynskiy) and pellets (Victoria), as well as a number of other fields of interest in the production of thermal insulation materials (Aysor, Alexandrov, Sergeev, Toguzak-Shulgin, Sarbai, Novotroitsk, Davydenovsk, Kamennoozernoe, Zhilandinsk, Zhangeldinsk, Alechinsky, Zhurunsk, Kenaralsk).

Spongolite deposits in Central Kazakhstan have restricted distribution only in the Pavlodar region (Mysore, Ekibastuz, Aktogay). They are confined to nizhnepaleogenovym deposits. conducting exploration is recommended for the identification of new projects.

On the territory of South Kazakhstan region recorded more than 20 deposits and occurrences opoks and opoka-like clay to mark the Suzak and hanavat tiers paleogene. Opoka-like breed developed in areas Kyngrak, Darbaza, Zhilgin and other domed uplifts paleogene.

The Turkestan deposit is located in Turkestan district, 30 km north-east of the city of Turkestan. A.V. Barbot de Marni studied in 1933. Deposits represented by alternating layers of opoks (capacity of 0.3-1.8 m) and opoka-like clay (thickness of 0.1-2 m).

The chemical composition of the opoks and opoka-like clays are shown in Tables 1 and 2.

Table 1 - Chemical composition of opoks

Oxides content,% by weight
SiO2	Al2O3	CaO	MgO	SO3	LOI
65,86-80,0	10,4-14,48	1,02-7,6	1,17-2,4	0,45-3,34	3,49-11,59

Table 2 - Chemical composition opoka-like clay

Oxides content,% by weight
SiO2	R2O3	CaO + MgO
65	15	> 10

Volumetric opoks weight - 1.35 g / cm³, the activity on the absorption of CaO - 300-396 mg / g. The field's reserves in categories A + B + C₁ account for more than 0.17 million tons.

The Turkestan II deposit is located in the Turkestan district, 18 km north-east of the city of Turkestan. He studied in 1937 A.V.Barbot-de-Marne.

Middle eocene reservoir opoks form three occurring in the subsurface sandstones, conglomerates are underlain by the same age. The power of the upper reservoir 0,3-1,75 m, middle and lower reaches 0,7-1,8 m.

The chemical composition of the opoks contained in Table 3 below.

Table 3 - Chemical composition of opoks

Oxides content,% by weight
SiO2	Al2O3	CaO	MgO	SO3	LOI
62,6-78,8	13,28-14,8	7,6-1,5	1,17-1,52	0,6-3,34	4,5-11,5

Volumetric opoks mass - 2,2-2,52 g / cm³ and a water absorption - 3,2-35,8%. The field's reserves in categories A + B comprise 0.2 million tons.

Kyngrak deposit located in Saryagash district, a 5 - 6 km to the north of n Kaplanbek. He studied in 1943-44 G.A. Voronov and others.

Productive stratum paleocene-eocene represented opoks, which are deposited in the form of small lenses capacity of 0,6-5,6 m, prisoners among opok-like clays, which power 1,1-6,2 m. Opok-like clay traced a narrow strip of the size of 2000 x 150 m around the dome. Activity rocks on the absorption of CaO - 170-313,5 mg / g. Reserves of C₂ category - more than 0.5 million tons.

Darbaza deposit located in Saryagash district, 1.5 km south of the w/d st. Darbaza studied in 1952 A.I. Voronov.

Productive stratum paleocene-eocene represented by interbedded clays and opoka-like clay. Active absorption rocks CaO - 206-352 mg/g. The field's reserves more than 0.35 million tons.

Darbazinskoe deposit (sections Darbaza and Central) is located in Saryagash district, 5 km south of the w/d st. Darbaza. Studied in 1954, 1957-59 A.I. Voronov.

Productive stratum paleocene-eocene represented opoka-like alternation of clays and clay opoks. Power 0,7-4,5m horizon.

Chemical composition opoks and opoka-like clay contained in the following Tables 4 and 5.

Table 4 - Chemical composition of opoks

Oxides content,% by weight
SiO2	Al2O3	Fe2O3	TiO2	CaO	MgO	Na2O	K2O	SO3	Н2О	LOI
69,97-78,63	6,11-10,38	2,37-3,44	0,25-0,45	0,3-2,19	0,98-1,82	0,55-1,07	0,69-1,12	0,76-3,75	3,34-4,36	3,97-6,53

Table 5 – Chemical composition opoka-like clay

Oxides content,% by weight
SiO2	Al2O3	Fe2O3	TiO2	CaO	MgO	Na2O	K2O	SO3	Н2О	LOI
60,96-68,07	7,14-12,1	2,96-4,48	0,4-0,5	1,02-3,72	1,18-2,18	0,35-0,99	0,78-1,42	1,32-5,22	-	5,05-8,01

Activity on the absorption opoks of lime - 600 mg / g, and opoka-like clay 150 mg / g. Stocks opoks deposits account for about 0.15 million tons.

Shymkent deposit located 10 km south-west of the city of Shymkent. He studied in 1961 M.S. Galiev.

Opoka-like clay, the power of which 1.4 m, occur among the greenish-gray paleocene - eocene bentonite clays.

Chemical composition opoka-like clay is given in the following table 6.

Table 6 - Chemical composition opoka-like clay

Oxides content,% by weight
SiO2	TiO2	Al2O3	FeO	Fe2O3	Mn	P2O5	CaO	MgO	SO3	K2O	Na2O	Н2О	LOI
75,12	0,35	7,91	0,14	2,25	0,005	0,46	3,28	1,74	0,14	0,91	1,6	2,22	4,64

The Zhausumkum deposit is located in Shardara district, on Shardara deposit area of bentonite clays (Yu.A.Alehin).

Productive stratum is represented opoks Suzak tier paleogene capacity of 1 m. The chemical composition of the opoks is provided in the following Table 7.

Table 7 - The chemical composition of the opoks

Oxides content,% by weight
SiO2	Al2O3	Fe2O3	TiO2	CaO	MgO	Na2O+ K2O	SO3	Н2О	LOI
78,3	7,33	2,23	0,12	1,78	0,48	1,6	0,35	4,36	2,84

Humidity opoks - 8.95, relative density - 2.4 g / cm³, the volumetric weight - 1.41 tonn / m³, the activity - from 356.68 to 395.38 mg / g. Stocks opoks deposit amount to category C₂ more than 30 thousand m³.

The field Turkestan-Urangay is located Turkestan in an area 15 kilometers north-east of the city of Turkestan, 4 km north-east of p.Urangay (Yuri Alekhin).

Productive stratum is represented opoks and paleogene opoka-like clays and have a capacity of 0.5-5.5 m. Opoks have a high water absorption. Stocks opoks and opoka-like clay is 8 million m³.

Manifestation Zhilginskoe located in Saryagash district, 3-4 km south-east of the w/d st. Zhilga (Yuri Alekhin).

Productive stratum is represented opoks Suzak tier paleogene capacity of 1.8 m opoks activity - 150 to 350 mg / g. Inventories are not counted.

Working process

To determine the average grindability sample opoks must be broken first in laboratory jaw (Figure 1a), then in a roll crusher (Figure 1b) and passed through a sieve with a hole diameter of 10 mm. To test flasks residues should be selected on the screen with a hole diameter of 5 mm.

a)	b)

a) – Jaw, inlet 150-100 mm, 20-50 mm output

b) – roller, inlet 20-50 mm, 10-15 mm output

Figure 1 - Laboratory Crushers

This residue the opoks in an amount of 1 kg is necessary in a laboratory mill grind ML-1r (Figure 2a), the loaded set range grinding metal balls 20 mm in diameter in an amount of 10 kg for 0, 15, 30, 45 and 60 minutes. After each grinding is necessary to take samples for analysis and sieving into fractions by sieves №5000, 3150, 2000, 1000, 500, 315, 100 μm using a vibrating screen Fritsch Analysette 3 PRO (figure 2b).

а)	b)

a) – Laboratory roller mill MLR-15;

b) – Circular Vibrating Screen Fritsch Analysette 3 PRO

Figure 2 - The Mill and crashing the laboratory

These sieving into fractions of ground opoks is necessary to bring the table 8.

Table 8 - Data sieving into fractions

Material	Time, min	Sieve size, μm
		5000	3150	2000	1000	500	315	100	<100	Σ
		%	%	%	%	%	%	%	%	%
Opoks	0
	15
	30
	45
	60

To a mixture of foaming is necessary to use preformed metal molds with the dimensions 5x5x5 cm, internal walls are deposited clay layer to prevent lubricant during heat treatment sample adhesion to the mold, and themselves form a metal tray placed on backfilling with alumina.

The prepared mixture is necessary to form a uniformly load, filling 40-45% of their volume, and to manually seal the mixture. Then move the form into a preheated to 600⁰C electric muffle furnace for foaming (Figure 3).

Figure 3 - Electric muffle furnace

In the chamber of the furnace must be installed in the form of constant temperature zone. Next, heat treatment is necessary to bring 850⁰C temperature for 40-50 minutes. The rate of temperature rise 6-8⁰C / min. At this temperature the samples must stand for 30 minutes. This delay is necessary to obtain a foamed mass. To fix the foam in the furnace temperature drastically reduced, thus opening a short distance oven door.

In the final step the samples were subjected to annealing - slow process of spontaneous cooling in the furnace from 850⁰C to 50⁰C temperature for 18-20 hours. This is due to the need to prevent thermal stresses during cooling.

Technological calculations

After removing the samples from the forms they impart predetermined size by trimming the edges. Next, determine the properties of the samples.

Techniques for determining the properties of foamed glass samples.

Density determination

To determine the density of the obtained foam glass samples using the following tools and instruments:

- electronic scales

- caliper

Beginning on electronic scales determined by the mass of samples, then a caliper to measure the length, width and height of the volume of the samples were found.

According to the formula , calculate the density of the obtained samples.

Determination of water absorption by volume

To determine water absorption foam glass samples obtained using the following devices:

• electronic scales

• electric tile

• thermoglasses

First electronic scales determine the mass of samples, the samples then immersed in boiling water on a hot plate thermoglasses for 1 hour. Samples should be completely submerged in water. After they are removed, wipe with a damp cloth and weighed on electronic scales.

According to the formula , find the average weight,

where: m₁ – weight before boiling in water, g

m₂ – weight after boiling in water, g

According to the formula , %, calculate the water absorption of the obtained samples

Determination of total (true) porosity

You need to know the size and weight of the samples to determine the porosity of the resulting foam glass samples, as well as the density of the mixture.

According to the formula , we find pore volume

where: m – the mass of the original sample, g

ρ – density of the mixture, g/sm³

Vsample – initial sample volume, sm³

and from here the formula , %, calculate the porosity of the obtained samples.

The density of the mixture is determined by hydrostatic weighing according to formula ,

where: ρ – density of the mixture, g/sm³

m – sample weight in air, g

m₁ – sample weight in liquid, g

ρf – density of the fluid at the test temperature, g/sm³

ρa – air density at the test temperature, g/sm³

Determination of open porosity

To determine the open porosity of the resulting foam glass samples measured weight of the sample after water absorption.

According to the formula , %, calculating open porosity obtained samples

where: m₁ – the mass of the original sample, g

m₂ – mass of the sample after boiling, g

V_обр – initial sample volume, sm³

Determination of closed porosity

To determine the closed porosity of the resulting foam glass samples need to know the total and open porosity samples.

According to the formula , %, calculating a closed porosity of the obtained samples

The results are recorded in Table 9.

Table 9 – Preparation of foam glass powder method

Composition of charge	The temperature and foaming time	Coefficient of foaming	Characteristics of the foam glass
			Density, g / cm3	Water uptake %	Porosity, %

The order of registration reports and their protection:

The report is issued in the following order:

1. To familiarize with the procedure of GOST 16381 - 77. Building materials and products insulating. Classification and general technical requirements.

2. To familiarize with the procedure of GOST 17177 - 94. Building materials and products insulating. Test methods.

3. Read the method of GOST (STB) 1322 - 2002 blocks of insulating foam glass. Specifications.

4. To study the physical and mechanical, chemical and physical properties of natural siliceous materials

5. Assess the suitability of raw materials for the thermal insulation foam glass technology building purpose

6. Carry out firing and receiving flask foam glass thermal insulation of building purpose

Control questions

1. To characterize the natural siliceous raw materials?

2. To characterize opoks?

3. To characterize foam glass?

Home setting:

1. To familiarize with the procedures of GOST 16381 - 77. Building materials and products insulating. Classification and general technical requirements. GOST 17177 - 94. Building materials and products insulating. Test methods. GOST (STB) 1322 - 2002 blocks of insulating foam glass. Specifications.

2. Carry out an analytical review of the natural siliceous raw materials for the South Kazakhstan region

3. To study the physical and mechanical, physical and chemical properties of natural siliceous materials

4. Carry out an analytical review of the market of building materials and thermal insulation of the Republic of Kazakhstan

Assignments for MIW