CN110204234B - Preparation method of double-shell hollow large granule material - Google Patents

Preparation method of double-shell hollow large granule material Download PDF

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CN110204234B
CN110204234B CN201910334195.6A CN201910334195A CN110204234B CN 110204234 B CN110204234 B CN 110204234B CN 201910334195 A CN201910334195 A CN 201910334195A CN 110204234 B CN110204234 B CN 110204234B
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water
shell
double
shell layer
strengthening solution
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庞超明
孟鑫鑫
徐剑
郦培娟
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Nanjing Tumu Energy Saving Technology Co ltd
Southeast University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/02Loose filtering material, e.g. loose fibres
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00Biological treatment of water, waste water, or sewage
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B20/00Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/10Coating or impregnating
    • C04B20/12Multiple coating or impregnating
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K21/00Fireproofing materials
    • C09K21/14Macromolecular materials
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00Biological treatment of water, waste water, or sewage
    • C02F2003/001Biological treatment of water, waste water, or sewage using granular carriers or supports for the microorganisms

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  • Life Sciences & Earth Sciences (AREA)
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Abstract

本发明公开了一种双壳层中空大颗粒料的制备方法,采用可吸水膨胀的树脂作为内核,树脂内核先预吸收大部分的水分,制备添加有少量短纤维的内壳层强化溶液,供已接近饱和的树脂内核吸收,并在树脂内核表面形成纤维网,形成内壳层;采用成球工艺,在表面包裹可形成强度的胶结材料;待材料硬化形成强度后,颗粒再次经过具有粘度的含渗透材料的溶液,让颗粒外层表面形成一个硬壳层;采用烘干的方式进行养护,使吸水树脂的水分完全放出,形成热养护,并形成中空。所制备的双壳层颗粒料具有良好的抗跌落性能,兼具比强度高,保温隔热性能好、耐火性高、抗裂性好等特点。

Figure 201910334195

The invention discloses a method for preparing a double-shell hollow large particle material. A water-swellable resin is used as a core, and the resin core first absorbs most of the water to prepare a strengthening solution for the inner shell added with a small amount of short fibers. The resin core that has been nearly saturated is absorbed, and a fiber network is formed on the surface of the resin core to form an inner shell layer; a spheroidizing process is used to wrap the surface with a bonding material that can form strength; after the material hardens to form strength, the particles pass through the viscosity The solution containing the permeable material forms a hard shell layer on the outer surface of the particles; curing is carried out by drying, so that the water of the water-absorbing resin is completely released, forming thermal curing, and forming a hollow. The prepared double-shell granules have good anti-drop performance, high specific strength, good thermal insulation performance, high fire resistance, good crack resistance and the like.

Figure 201910334195

Description

Preparation method of double-shell hollow large granule material
Technical Field
The invention belongs to the field of environment treatment and building heat insulation materials, and also can be used for agricultural ridging materials, in particular to a preparation method of a double-shell hollow large granule material.
Background
In recent years, along with the increasing global water pollution, biofilters are widely applied in sewage treatment processes. The ceramsite is a porous substance with a rough surface as a filter material, has good microorganism adhesiveness and certain adsorption capacity, and can be widely applied to water treatment as a biological filter material and a substrate.
At present, a patent product CN 103496866B is available, and the disclosed core-shell type baking-free lightweight aggregate is used as a baking-free ceramsite and is already applied to the aspects of building heat preservation and environmental treatment, but the core-shell type baking-free lightweight aggregate has poor toughness and is easy to damage and leak the EPS core by a forklift when being used in bulk; if the porous material is used as a filter material, the total porosity of particles is low due to the existence of the inner core, and the filtering capability is insufficient. The patent product CN 102936127 a discloses a sintered lightweight hollow ceramsite, which is obtained by removing EPS nuclei in the ceramsite to be hollow by sintering, but this way of preparing the ceramsite has high energy consumption and poor toughness. The Liaoning architecture professional college Huanglihua research prepares a multi-shell baking-free ceramsite, but the baking-free ceramsite has high density, low specific strength, low porosity and water absorption, and insufficient filtering capability if used as a biological filter material.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a double-shell hollow large granule, and the prepared double-shell hollow large granule has the characteristics of high crack resistance, light weight, high specific strength (strength under unit density, namely high strength under the same density or low density under the same density), good toughness, good heat insulation performance, good fire resistance and the like, is hollow, has high porosity and has good filtering capacity.
The technical scheme of the invention is as follows:
a preparation method of a double-shell hollow large granule material comprises the following steps:
step 1), taking water-absorbent resin particles as a core, and carrying out pre-water saturation treatment on the water-absorbent resin particles, wherein the water saturation degree is controlled to be 75-90%;
step 2) preparing an inner shell layer strengthening solution, placing the water-absorbent resin which is saturated by water and is prepared in the step 1) into the inner shell layer strengthening solution, and stirring;
step 3) selecting a silicate cement-based material or a phosphate cement-based material as a cementing material, and wrapping the water-absorbing resin treated in the step 2) and the cementing material into a shell by adopting a balling process;
step 4) naturally curing the water-absorbing resin wrapped into the shell prepared in the step 3) for 1-4 h;
step 5) preparing a shell layer strengthening solution, and spraying the shell layer strengthening solution on the surface of the cured material prepared in the step 4);
and 6) sealing, drying and maintaining the material treated in the step 5) to obtain the material.
Preferably, the particle size of the water-absorbent resin which is saturated with water is 2-7 mm.
Preferably, the inner shell layer strengthening solution consists of the following raw materials in percentage by weight: 10-30% of sodium silicate, 0.5-5% of silicon dioxide powder, 5-30% of industrial starch, 0.5-2% of fiber material and the balance of water.
Preferably, the fiber material is polypropylene fiber with the length of 2-3 mm.
Preferably, the shell layer strengthening solution consists of the following raw materials in percentage by weight: 5-20% of sodium silicate, 0-3% of silicon dioxide powder and the balance of water.
Preferably, the drying and curing temperature in the step 6) is 100-150 ℃.
The invention has the following advantages:
(1) the water-absorbent resin is used as a core material, and the core material does not contain inflammable substances, so that the fire resistance of the aggregate is effectively improved. On one hand, the inner core of the water-absorbent resin is dehydrated by adopting a drying and maintaining mode at 100-150 ℃, so that a hollow structure is formed, and the density is reduced; on the other hand, the inside evaporated moisture can make the shell material form sufficient steam curing, which is beneficial to improving the specific strength of the large-particle material.
(2) The solution containing the reinforcing material is used as the later-stage absorption liquid of the water-absorbent resin, so that the specific strength of the aggregate can be improved, and the early-stage conveying of the aggregate is facilitated.
(3) The reinforcing material of the inner shell layer is doped with fibers, so that the characteristics of early brittleness and easy cracking of the aggregate can be obviously improved.
(4) The outer layer is also made of solution containing reinforcing material, and the solution containing penetrating material is sprayed or roll-coated on the particles to form a hard shell layer on the surfaces of the particles.
(5) The inner core is resin, if the inner core is used as a building heat-insulating material, the inner core cannot burn due to the absence of oxygen at high temperature, and the inner core needs to absorb heat when the inner core is melted, so that the propagation speed of heat is reduced, and the spreading speed of fire is relieved.
(6) The prepared double-shell hollow large-particle material has high porosity, and the high porosity can ensure good heat insulation performance, and can obviously improve the heat insulation performance of a product when being used in a heat insulation product; the water absorption rate of the material can be effectively improved, and can reach over 17% through detection, and the water filtering capacity is strong.
Drawings
FIG. 1 is a flow chart of a preparation method of a double-shell hollow large granule material;
FIG. 2 is a diagram of a finished product of a double-shell hollow large granule material;
FIG. 3 is a cross-sectional view of a double-shell hollow macroparticle;
FIG. 4 is a partially enlarged cross-sectional view of a double-shell hollow macroparticle.
Detailed Description
The invention is further illustrated with reference to the accompanying drawings and specific embodiments.
Example 1
A preparation method of a double-shell hollow large granule material is shown in figure 1, and the selected materials and steps are as follows:
(1) a water-absorbent resin having a diameter of 6mm after water absorption was used as the inner core, and the water retention level of the water-absorbent resin was controlled to 75% in advance.
(2) Preparing an inner shell layer strengthening solution, adopting a 30% sodium silicate solution, and adding 2% of silicon dioxide powder and 0.5% of polypropylene fibers (the length is 2-3 mm).
(3) Placing the water-absorbent resin which is saturated with water into the inner shell layer strengthening solution, and slowly stirring for 1 min.
(4) The Portland cement with the components of 40 percent, 20 percent of mineral powder and 40 percent of fly ash are used as cementing materials (1-1 group); or the components are 75 percent of phosphate cement and 25 percent of fly ash as the cementing material (1-2 groups).
(5) Putting the pretreated water-absorbing resin and the cementing material into a balling disc together to wrap the powder into balls.
(6) Preparing a shell layer strengthening solution by using a 5% sodium silicate solution.
(7) Naturally curing the balled material for 4h (1-1 group) or 1h (1-2 group), placing the cured material in a rotary drum, and atomizing and spraying a shell layer strengthening solution.
(8) Sealing, and curing in a 110 deg.C oven.
The properties of the prepared products are shown in groups 1-1 and 1-2 in Table 1.
Example 2
A preparation method of a double-shell hollow large granule material is shown in figure 1, and the selected materials and steps are as follows:
(1) a water-absorbent resin having a diameter of 6mm after water absorption was used as the inner core, and the water retention level of the water-absorbent resin was controlled to 75% in advance.
(2) Preparing an inner shell layer strengthening solution, adopting a 10% sodium silicate solution, and adding 5% industrial starch and 2% polypropylene fiber (the length is 2-3 mm).
(3) Placing the water-absorbent resin which is saturated with water into the inner shell layer strengthening solution, and slowly stirring for 1 min.
(4) Phosphate cement with the components of 90 percent and fly ash silica-based material with the components of 10 percent are adopted as cementing materials (group 2-1); or the components of 50 percent of Portland cement and 50 percent of fly ash silica-based material are used as the cementing material (group 2-2).
(5) Putting the pretreated water-absorbing resin and the cementing material into a balling disc together to wrap the powder into balls.
(6) Preparing a shell layer strengthening solution, adopting a 20% sodium silicate solution, and adding 3% silicon dioxide powder.
(7) Naturally curing the balled material for 1h (2-1 group) or 4h (2-2 group), placing the cured material in a screw conveyor, and atomizing and spraying a shell layer strengthening solution.
(8) Sealing, and curing in a 110 deg.C oven.
The properties of the prepared products are shown in groups 2-1 and 2-2 in Table 1.
TABLE 1 Properties of the double-shelled hollow macroparticles
Figure BDA0002038643540000041
As can be seen from Table 1, the successfully prepared double-shell hollow large-particle material has the advantages of light weight, large porosity, high water absorption, strong water filtration capacity and certain strength, and can be well applied to biological filter materials. The macroporosity can ensure good heat insulation performance, and when the material is used in a heat insulation product, the heat insulation performance of the product can be obviously improved; the water absorption of the material can be effectively improved and can reach more than 17% through detection. The finished product is shown in figures 2, 3 and 4.
The above description is only a part of the implementation method of the present invention, and it should be noted that: it will be apparent to those skilled in the art that several contemplated modifications and adaptations can be made without departing from the principles of the invention and these are intended to be included within the scope of the invention.

Claims (4)

1.一种双壳层中空大颗粒料的制备方法,其特征在于,包括以下步骤:1. a preparation method of double-shell hollow large granular material, is characterized in that, comprises the following steps: 步骤1)将吸水树脂颗粒作为内核,对其进行预饱水处理,饱水程度控制在75~90%;Step 1) using the water-absorbent resin particles as the inner core, and carrying out pre-saturated water treatment, and the water saturation degree is controlled at 75-90%; 步骤2)配置内壳层强化溶液,将步骤1)制得的已吸水饱和的吸水树脂置于内壳层强化溶液中,搅拌;Step 2) configuring the inner shell layer strengthening solution, placing the water-absorbent saturated water-absorbent resin obtained in step 1) in the inner shell layer strengthening solution, and stirring; 所述内壳层强化溶液由以下原料按重量百分比组成:10~30%的硅酸钠、0.5~5%的二氧化硅粉、5~30%的工业淀粉、0.5~2%的纤维材料,其余为水;The inner shell strengthening solution is composed of the following raw materials by weight percentage: 10-30% sodium silicate, 0.5-5% silicon dioxide powder, 5-30% industrial starch, 0.5-2% fiber material, The rest is water; 步骤3)选择硅酸盐水泥基材料或磷酸盐水泥基材料作为胶结材料,将经步骤2)处理的吸水树脂与胶结材料采用成球工艺包裹成壳;Step 3) Select Portland cement-based material or phosphate cement-based material as the cementing material, and wrap the water-absorbing resin and cementing material processed in step 2) into a shell by a ball-forming process; 步骤4)对步骤3)制得的包裹成壳的吸水树脂进行自然养护1~4h;Step 4) carrying out natural curing for the water-absorbent resin wrapped into a shell prepared in step 3) for 1-4 hours; 步骤5)配置外壳层强化溶液,对步骤4)制得的已养护的材料表面喷洒所述外壳层强化溶液;Step 5) configure the shell layer strengthening solution, and spray the shell layer strengthening solution on the surface of the cured material obtained in step 4); 所述外壳层强化溶液由以下原料按重量百分比组成:5~20%的硅酸钠、0~3%的二氧化硅粉,其余为水;The outer shell layer strengthening solution is composed of the following raw materials by weight percentage: 5-20% of sodium silicate, 0-3% of silicon dioxide powder, and the rest is water; 步骤6)对经步骤5)处理的材料进行密闭,烘干养护,即得。Step 6) Sealing the material processed in step 5), drying and curing, that is, it is obtained. 2.根据权利要求1所述的一种双壳层中空大颗粒料的制备方法,其特征在于,所述已吸水饱和的吸水树脂的粒径为2~7mm。2 . The method for preparing a double-shell hollow large particle material according to claim 1 , wherein the particle size of the water-saturated water-absorbing resin is 2-7 mm. 3 . 3.根据权利要求1所述的一种双壳层中空大颗粒料的制备方法,其特征在于,所述纤维材料为聚丙烯纤维,长度2~3mm。3 . The method for preparing a double-shell hollow large particle material according to claim 1 , wherein the fiber material is polypropylene fiber with a length of 2-3 mm. 4 . 4.根据权利要求1所述的一种双壳层中空大颗粒料的制备方法,其特征在于,步骤6)所述烘干养护的温度为100~150℃。4 . The method for preparing a double-shell hollow large granular material according to claim 1 , wherein the drying and curing temperature in step 6) is 100-150° C. 5 .
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CN110683860B (en) * 2019-11-18 2021-10-22 萍乡学院 A kind of ceramic hollow sphere with double shell structure and preparation method thereof
CN113173722A (en) * 2021-03-31 2021-07-27 恒尊集团有限公司 Sintering-free lightweight aggregate, preparation method thereof and lightweight concrete

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CN108892441A (en) * 2018-03-26 2018-11-27 武夷山德邦环保节能设备制造有限公司 Using hollow concrete ball as functional material permeable terrace construction technique

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CN1332767A (en) * 1998-11-05 2002-01-23 三井化学株式会社 Particle containing crosslinked polyamino acid
CN107614581A (en) * 2011-04-13 2018-01-19 希提米克斯公司 Lightweight synthesis particle and the method for manufacturing lightweight synthesis particle
CN102492175A (en) * 2011-11-08 2012-06-13 中国科学技术大学 Microcapsule flame-retardant adsorption resin and preparation method thereof, and flame-retardant composite material
CN103496866A (en) * 2013-09-23 2014-01-08 东南大学 Preparation method of novel core-shell type cement-based high-strength lightweight aggregate
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CN108892441A (en) * 2018-03-26 2018-11-27 武夷山德邦环保节能设备制造有限公司 Using hollow concrete ball as functional material permeable terrace construction technique

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