WO2021056638A1 - 一种复合保温隔热材料及其制备方法 - Google Patents
一种复合保温隔热材料及其制备方法 Download PDFInfo
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- WO2021056638A1 WO2021056638A1 PCT/CN2019/111834 CN2019111834W WO2021056638A1 WO 2021056638 A1 WO2021056638 A1 WO 2021056638A1 CN 2019111834 W CN2019111834 W CN 2019111834W WO 2021056638 A1 WO2021056638 A1 WO 2021056638A1
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- thermal insulation
- insulation material
- diatomite
- composite thermal
- cement
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/40—Porous or lightweight materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Definitions
- the invention relates to a composite thermal insulation material and a preparation method thereof, in particular to a cement-based silica aerogel-diatomite composite thermal insulation material and a preparation method thereof, and belongs to the field of thermal insulation materials.
- silica aerogel is currently the lowest-density solid material that is a research hotspot in thermal insulation.
- the traditional preparation method uses organic solvents as raw materials and is prepared by supercritical drying.
- the equipment cost is high, the parameter control is complicated, the time-consuming is long, the continuous production is not possible, and the flammable and toxic solvent vapor may be released during the process, and the safety is low.
- atmospheric drying and cheap preparation have become new research hotspots.
- the quality of silica aerogels under atmospheric drying needs to be improved. It is easy to crack and shrink, have many by-products, waste a lot of solvent, and the solvent replacement process takes a long time.
- the purpose of the present invention is to provide a composite thermal insulation material and a preparation method thereof, specifically to provide a cement-based silica aerogel-diatomite composite
- the thermal insulation material and its preparation method have simple process, low cost, easy industrial production and certain strength, which overcomes the shortcomings of silica aerogel that cannot be used in large quantities in the construction industry due to its high price and low strength. Adjusting the indoor temperature can greatly reduce the thermal conductivity of cement-based materials and greatly save energy.
- the present invention provides a composite thermal insulation material, which is a cement-based silica aerogel-diatomite composite thermal insulation material, and includes the following components in parts by mass:
- the specific surface area of the silica aerogel without diatomite is ⁇ 400m 2 /g, and the diatomite is ultrafine diatomite with a particle size of ⁇ 300 mesh .
- the length of the polypropylene fiber is between 6 mm and 12 mm, and the coupling agent is a liquid silane coupling agent.
- the cellulose ether is a solid powder of hydroxypropyl methylcellulose with a viscosity of 100,000 to 200,000 MPa ⁇ s and a sieving rate of 80 mesh ⁇ 98%; the redispersible latex powder is a solid powder with a sieve with a diameter of 400um. The amount is less than or equal to 4%, and the solid content is ⁇ 99%.
- the room temperature thermal conductivity of the cement-based silica aerogel-diatomite composite thermal insulation material ranges from 0.13 to 0.27 W/(m ⁇ K), and the compressive strength ranges from 3 to 5 MPa.
- the present invention provides a method for preparing a composite heat preservation and heat insulation material.
- the method includes the following steps:
- step 1) the mixing and grinding of fly ash and sodium carbonate refers to the mixing and grinding of fly ash and sodium carbonate in a mass ratio of 1:0.8 to 1:1.5 to less than 200 mesh.
- Step 1) The particle size of the fly ash is passed through a 200 mesh sieve; Step 1)
- the high-temperature calcination treatment refers to a high-temperature calcination treatment at a temperature of 750-850°C for 1.5-2h.
- the feasible acid in step 2) is sulfuric acid, hydrochloric acid, hydrofluoric acid, phosphoric acid, oxalic acid or nitric acid; in step 2), the adjusting reagent used in the subsequent adjustment of pH to 3-7 is ammonia water, and the standing in step 2)
- the aging time is 1d ⁇ 2d.
- Step 6 When adding water and mixing uniformly, the quality of the added water is 1 to 2 times the quality of the cement.
- the present invention has the following advantages:
- the cement-based silica aerogel-diatomite composite thermal insulation material provided by the present invention is prepared by preparing a silica wet gel with fly ash and embedding it in diatomaceous earth through classification and drying, which overcomes Organic thermal insulation materials are flammable and traditional inorganic thermal insulation materials have relatively high thermal conductivity shortcomings. At the same time, it overcomes the shortcomings of complex preparation process of silica aerogel, high raw material cost and small application range.
- silica aerogel is used as the thermal insulation material
- diatomaceous earth is used as the support material of the silica aerogel
- the thermal insulation material is introduced into the cement material to prepare the cement-based silica Aerogel-diatomite composite thermal insulation material has low thermal conductivity and good thermal insulation performance. Its thermal conductivity decreases with the increase of thermal insulation material silica aerogel.
- the mechanical properties of the cement-based silica aerogel-diatomite composite thermal insulation material of the present invention make up for the good thermal insulation performance of the existing silica aerogel thermal insulation material, but the strength is too low,
- the high cost defect, the strength of the cement-based silica aerogel-diatomite composite thermal insulation material decreases with the increase of the thermal insulation material content, and the minimum is 3MPa, which meets the mechanical performance requirements of masonry mortar buildings and makes up for it.
- the existing silica aerogel thermal insulation materials have the defect of good thermal insulation performance but too low strength.
- the preparation of the cement-based silica aerogel-diatomite composite thermal insulation material of the present invention has a wide range of raw materials, low preparation cost, overcoming the high cost defects in the prior art, and the preparation method is simple in equipment and operation. Convenient and easy to industrialized production.
- Figure 1 is a scanning electron micrograph of the surface morphology of the raw material diatomaceous earth and the silica aerogel-diatomite materials in Examples 1 to 4, where a is diatomaceous earth, and b, c, and d are examples 1 to in sequence.
- the prepared silica aerogel-diatomite material, e and f are the silica aerogel-diatomite material prepared in Example 4;
- Figure 2 is a graph showing the nitrogen adsorption and desorption curves of diatomaceous earth as a raw material and the silica aerogel-diatomite materials in Examples 1 to 4;
- Fig. 3 is an XRD test diagram of diatomaceous earth as a raw material, silica aerogel prepared without adding diatomaceous earth, and silica aerogel-diatomite materials prepared in Examples 1, 2, and 4;
- Figure 4 is the FT-IR test diagram of the raw material diatomaceous earth, the silica aerogel prepared without adding diatomaceous earth, and the silica aerogel-diatomite material prepared in Examples 1, 2 and 4 ;
- Fig. 5 is a thermal conductivity analysis diagram of cement paste test block, 1#-9# prepared in Examples 1-9, where a is cement paste test block, 1#-4# prepared in Examples 1 to 4
- the thermal conductivity analysis diagram of, b is the cement paste test block, the thermal conductivity analysis diagram of 5#-9# prepared in Examples 5-9;
- Fig. 6 is a graph showing the compressive strength performance analysis of cement paste test block, 1#-9# prepared in Examples 1-9, where a is cement paste test block, 1# ⁇ prepared in Examples 1-4 4# compression performance analysis diagram, b is the cement paste test block, the compression performance analysis diagram 5#-9# prepared in Examples 5-9;
- Fig. 7 is a preparation flow chart of cement-based silica aerogel-diatomite composite thermal insulation material.
- a composite thermal insulation material (1#) is a cement-based silica aerogel-diatomite composite thermal insulation material, and includes the following components in parts by mass:
- the coupling agent is a liquid silane coupling agent
- the redispersible latex powder is a solid powder
- the polypropylene fiber length is between 6mm and 12mm
- the cellulose ether is a solid powder hydroxypropyl Methyl cellulose has a viscosity of 100000 MPa ⁇ s.
- a method for preparing the above-mentioned composite thermal insulation material includes the following steps (as shown in Figure 7):
- a composite thermal insulation material (2#) is a cement-based silica aerogel-diatomite composite thermal insulation material, and includes the following components in parts by mass:
- the coupling agent is a liquid silane coupling agent
- the redispersible latex powder is a solid powder
- the polypropylene fiber length is between 6mm and 12mm
- the cellulose ether is a solid powder hydroxypropyl Methyl cellulose has a viscosity of 100000 MPa ⁇ s.
- a method for preparing the above-mentioned composite thermal insulation material includes the following steps (as shown in Figure 7):
- a composite thermal insulation material (3#) is a cement-based silica aerogel-diatomite composite thermal insulation material, and includes the following components in parts by mass:
- the coupling agent is a liquid silane coupling agent
- the redispersible latex powder is a solid powder
- the polypropylene fiber length is between 6mm and 12mm
- the cellulose ether is a solid powder hydroxypropyl Methyl cellulose has a viscosity of 100000 MPa ⁇ s.
- a method for preparing the above-mentioned composite thermal insulation material includes the following steps (as shown in Figure 7):
- the coupling agent is a liquid silane coupling agent
- the redispersible latex powder is a solid powder
- the polypropylene fiber length is between 6mm and 12mm
- the cellulose ether is a solid powder hydroxypropyl Methyl cellulose has a viscosity of 100000 MPa ⁇ s.
- a method for preparing the above-mentioned composite thermal insulation material includes the following steps (as shown in Figure 7):
- a composite thermal insulation material (#), the composite thermal insulation material is a cement-based silica aerogel-diatomite composite thermal insulation material, which includes the following components according to quality:
- the coupling agent is a liquid silane coupling agent
- the redispersible latex powder is a solid powder
- the polypropylene fiber length is between 6mm and 12mm
- the cellulose ether is a solid powder hydroxypropyl Methyl cellulose has a viscosity of 100000 MPa ⁇ s.
- a method for preparing the above-mentioned composite thermal insulation material includes the following steps (as shown in Figure 7):
- the coupling agent is a liquid silane coupling agent
- the redispersible latex powder is a solid powder
- the polypropylene fiber length is between 6mm and 12mm
- the cellulose ether is a solid powder hydroxypropyl Methyl cellulose has a viscosity of 100000 MPa ⁇ s.
- a method for preparing the above-mentioned composite thermal insulation material includes the following steps (as shown in Figure 7):
- the coupling agent is a liquid silane coupling agent
- the redispersible latex powder is a solid powder
- the polypropylene fiber length is between 6mm and 12mm
- the cellulose ether is a solid powder hydroxypropyl Methyl cellulose has a viscosity of 100000 MPa ⁇ s.
- a method for preparing the above-mentioned composite thermal insulation material includes the following steps (as shown in Figure 7):
- the coupling agent is a liquid silane coupling agent
- the redispersible latex powder is a solid powder
- the polypropylene fiber length is between 6mm and 12mm
- the cellulose ether is a solid powder hydroxypropyl Methyl cellulose has a viscosity of 100000 MPa ⁇ s.
- a method for preparing the above-mentioned composite thermal insulation material includes the following steps (as shown in Figure 7):
- the coupling agent is a liquid silane coupling agent
- the redispersible latex powder is a solid powder
- the polypropylene fiber length is between 6mm and 12mm
- the cellulose ether is a solid powder hydroxypropyl Methyl cellulose has a viscosity of 100000 MPa ⁇ s.
- a method for preparing the above-mentioned composite thermal insulation material includes the following steps (as shown in Figure 7):
- a composite thermal insulation material (10#) is a cement-based silica aerogel-diatomite composite thermal insulation material, and includes the following components in parts by mass:
- the coupling agent is a liquid silane coupling agent
- the redispersible latex powder is a solid powder
- the polypropylene fiber length is between 6mm and 12mm
- the cellulose ether is a solid powder hydroxypropyl Methyl cellulose has a viscosity of 100000 MPa ⁇ s.
- a method for preparing the above-mentioned composite thermal insulation material includes the following steps (as shown in Figure 7):
- a composite thermal insulation material (11#), the composite thermal insulation material is a cement-based silica aerogel-diatomite composite thermal insulation material, and includes the following components in parts by mass:
- the coupling agent is a liquid silane coupling agent
- the redispersible latex powder is a solid powder
- the polypropylene fiber length is between 6mm and 12mm
- the cellulose ether is a solid powder hydroxypropyl Methyl cellulose has a viscosity of 100000 MPa ⁇ s.
- a method for preparing the above-mentioned composite thermal insulation material includes the following steps (as shown in Figure 7):
- the coupling agent is a liquid silane coupling agent
- the redispersible latex powder is a solid powder
- the polypropylene fiber length is between 6mm and 12mm
- the cellulose ether is a solid powder hydroxypropyl Methyl cellulose
- viscosity is 200,000MPa ⁇ s.
- a method for preparing the above-mentioned composite thermal insulation material includes the following steps (as shown in Figure 7):
- a composite thermal insulation material (13#), the composite thermal insulation material is a cement-based silica aerogel-diatomite composite thermal insulation material, and includes the following components in parts by mass:
- the coupling agent is a liquid silane coupling agent
- the redispersible latex powder is a solid powder
- the polypropylene fiber length is between 6mm and 12mm
- the cellulose ether is a solid powder hydroxypropyl Methyl cellulose has a viscosity of 100000 MPa ⁇ s.
- a method for preparing the above-mentioned composite thermal insulation material includes the following steps (as shown in Figure 7):
- the cement-based silica aerogel-diatomite composite thermal insulation material (1#-13#) prepared in Examples 1-13 is off-white.
- the performance analysis of various parameters includes:
- Figure 1 is a scanning electron micrograph of the surface morphology of the raw material diatomaceous earth and the silica aerogel-diatomite materials in Examples 1 to 4, where a is diatomaceous earth, and b, c, and d are examples 1 to in sequence.
- the prepared silica aerogel-diatomite material, e and f are the silica aerogel-diatomite material prepared in Example 4; from the microstructure diagram, it can be seen that the diatomite is a porous cake
- the surface of the shape structure has a pore distribution similar to sieve pores. After the silica aerogel-diatomite material is formed, the pores of the diatomite become less and the specific surface area is greatly reduced. It can be seen from the figure that as the amount of diatomite increases, silica aerogel cannot completely fill the pores of diatomite, and some of the pores are exposed.
- Figure 2 is a graph showing the nitrogen adsorption and desorption curves of diatomaceous earth as a raw material and the silica aerogel-diatomaceous earth materials in Examples 1 to 4. It can be seen from the test results that the specific surface area of diatomaceous earth is relatively small, and the specific surface area of silica aerogel is known to be large. The maximum pore diameter of diatomaceous earth is about 4nm, and most of the micropores are visible from the nitrogen adsorption and desorption isotherm. As the mass ratio of diatomaceous earth to silica aerogel increases, the specific surface area of the silica aerogel-diatomite material changes from 554.465 m of the silica aerogel-diatomite material in Example 1.
- silica aerogel-diatomite material in Example 4 decreased to 84.009m 2 /g of the silica aerogel-diatomite material in Example 4, which is getting closer and closer to the specific surface area of diatomaceous earth, the pore diameter dropped to about 4nm, and the nitrogen adsorption and desorption isotherm was The characteristics of type I isotherm indicate that the silica aerogel-diatomite material is a microporous material, and the maximum pore size is about 2.2nm, which is consistent with the pore structure of silica aerogel.
- the dioxide Silica aerogel effectively fills the pores of diatomite and is effectively adsorbed under negative pressure to form a silica aerogel-diatomite material; as the amount of diatomite increases, silica aerogel-diatomite The specific surface area of the material is getting smaller and smaller, which is consistent with the analysis result of scanning electron microscopy.
- Fig. 3 is an XRD test diagram of diatomaceous earth as a raw material, silica aerogel prepared without adding diatomaceous earth, and silica aerogel-diatomite materials in Examples 1, 2, and 4. It can be seen from the figure that the peak intensity of silica aerogel-diatomite material is different, which is caused by the different content of diatomite in the silica aerogel-diatomite material. -Compared with the XRD patterns of diatomaceous earth materials and the XRD patterns of silica aerogels prepared without diatomaceous earth, no new peaks are produced, indicating that the invention adds diatomite negative pressure adsorption after the gel No new substances have been produced.
- Figure 4 is the FT-IR test diagram of the diatomite as the raw material, the silica aerogel prepared without adding diatomite, and the silica aerogel-diatomite materials in Examples 1, 2, and 4. It can be seen that the figure is the superposition of diatomaceous earth and silica aerogel. At the same time, it can be seen that there is no new peak shape. Therefore, the silica aerogel is mixed in the preparation process. The silica aerogel-diatomite material formed by adding diatomite does not generate new substances, the structure remains unchanged, and the thermal insulation material is stable.
- Figure 5 is a thermal conductivity analysis diagram of cement paste test blocks and 1#-9# prepared in Examples 1-9.
- Figure 5(a) is the analysis diagram of the thermal conductivity of the cement paste test block and Examples 1 to 4.
- FIG. 5(b) is the thermal conductivity analysis diagram of Examples 5-9. According to the above experimental results, with the increase of the amount of silica aerogel-diatomite material, the thermal conductivity varies from 5# to 8# It shows a decreasing trend, but the extent of the decrease is different; the thermal conductivity of Examples 5-9# increases greatly after water absorption, and water absorption has an adverse effect on the thermal conductivity.
- Fig. 6 is an analysis diagram of the compressive strength performance of cement paste test blocks and 1#-9# prepared in Examples 1-9.
- Figure 6(a) is the analysis diagram of the compressive performance of the cement paste test block and Examples 1 to 4.
- the compressive strength of cement-based silica aerogel-diatomite material is higher than that of pure cement
- the compressive strength of the test block has been greatly reduced, and the compressive strength of the cement-based composite test block after adding silica aerogel-diatomite material is significantly reduced.
- the silica aerogel-diatomite material With the increase of the content of medium diatomite, the compressive strength of 1# ⁇ 4# gradually increases.
- Figure 6(b) is the analysis diagram of the compressive strength performance of Examples 5-9.
- the compressive strength under wet conditions is about 13% lower than that under complete dry conditions.
- the minimum compressive strength under dry conditions is about 3MPa and the highest is After being saturated with water absorption, the compressive strength is in the range of 1.6 to 4.3 MPa.
- Fig. 7 is a preparation flow chart of cement-based silica aerogel/diatomite composite thermal insulation material.
- thermal insulation material of the present invention as a building thermal insulation material can effectively reduce the range of indoor and outdoor heat transfer in a building, reduce indoor temperature fluctuations, achieve indoor thermal insulation, reduce the use of building heating or air conditioning, and realize Building energy efficiency.
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Abstract
Description
Claims (10)
- 如权利要求1所述的一种复合保温隔热材料,其特征在于:所述的二氧化硅气凝胶-硅藻土材料中,不添加硅藻土时的二氧化硅气凝胶比表面积≥400m 2/g,硅藻土为粒径≤300目超细硅藻土。
- 如权利要求1所述的一种复合保温隔热材料,其特征在于:所述的聚丙烯纤维长度介于6mm~12mm之间,所述的偶联剂为液态硅烷偶联剂。
- 如权利要求1所述的一种复合保温隔热材料,其特征在于:所述的纤维素醚为固体粉末羟丙基甲基纤维素,粘度100000~200000MPa·s,80目过筛率≥98%;所述的可再分散乳胶粉为固体粉末,400um孔径筛筛余量小于等于4%,固含量≥99%。
- 如权利要求1所述的一种复合保温隔热材料,其特征在于:所述的水泥基二氧化硅气凝胶-硅藻土复合保温隔热材料的室温导热系数范围为0.13~0.27W/(m·K),抗压强度范围为3~5MPa。
- 一种如权利要求1~5任意所述的复合保温隔热材料的制备方法,其特征在于:该方法包括以下步骤:1)将粉煤灰与碳酸钠混合研磨,之后高温煅烧处理得到煅烧混合物;2)用可行酸水解煅烧混合物,之后调节PH至3~7之间,静置陈化后生成硅凝胶;3)依次用去离子水、乙醇多次洗涤硅凝胶,之后按照硅凝胶与硅藻土的质量比为1:1~1:5加入硅藻土,搅拌均匀后置于真空条件下进行负压吸附12h~48h至硅藻土完全进入凝胶中,得到复合材料;4)按照体积比8:1:1~8:2:1将正己烷、三甲基氯硅烷和乙醇混合配置得到 改性液,之后将复合材料浸泡在改性液中改性,每隔8~24h更换改性液直至复合材料悬浮或漂浮在改性液中后取出,用正己烷洗涤后得到改性复合材料;5)对改性复合材料进行分级干燥,室温~40℃干燥12~24h、100~130℃干燥2~4h,重复干燥直至恒重,得到二氧化硅气凝胶-硅藻土材料;6)按比例将二氧化硅气凝胶-硅藻土材料、水泥、聚丙烯纤维、偶联剂、纤维素醚和可再分散乳胶粉干拌均匀,之后加水搅拌均匀,得到所述的水泥基二氧化硅气凝胶-硅藻土复合保温隔热材料。
- 如权利要求6所述的一种复合保温隔热材料的制备方法,其特征在于:步骤1)所述的将粉煤灰与碳酸钠混合研磨,是指将粉煤灰与碳酸钠按照质量比1:0.8~1:1.5混合研磨至200目以下。
- 如权利要求6所述的一种复合保温隔热材料的制备方法,其特征在于:步骤1)所述的粉煤灰粒径过200目筛;步骤1)所述高温煅烧处理是指在750~850℃温度下高温煅烧处理1.5~2h。
- 如权利要求6所述的一种复合保温隔热材料的制备方法,其特征在于:步骤2)所述的可行酸为硫酸、盐酸、氢氟酸、磷酸、草酸或者硝酸;步骤2)所述的之后调节PH至3~7中所用调节试剂为氨水,步骤2)所述静置陈化时长为1d~2d。
- 如权利要求6所述的一种复合保温隔热材料的制备方法,其特征在于:步骤6)所述的加水搅拌均匀中,加入水的质量为水泥质量的1~2倍。
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