CN104402010A - Preparation method of xonotlite-type calcium silicate material - Google Patents
Preparation method of xonotlite-type calcium silicate material Download PDFInfo
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Abstract
The invention relates to a method of preparing a xonotlite-type calcium silicate material from active silicate dioxide and calcareous raw materials. The preparation method comprises the following steps: (1) individually grinding active silicon dioxide and calcareous raw materials so as to obtain active silicon dioxide powder and lime powder; (2) blending the active silicon dioxide powder and lime powder obtained in the step (1) according to a certain ratio, then transferring the mixture to a mixer with a stirring device, adding industrial water, evenly stirring to obtain a uniform material, after a moulding treatment or directly transferring the uniform material to an enclosed reactor, and controlling the temperature rising speed, the reaction temperature, and reaction time to carry out synthesis reactions; (3) moulding and/or drying the reaction products obtain in the step (2) so as to obtain the xonotlite-type calcium silicate material. The xonotlite-type calcium silicate material has the advantages of no toxicity, safety, low density, high strength, low heat conductive coefficient, and good chemical stability, and can be used in the industries such as electric power, chemical engineering, metallurgy, textile, building material, and the like.
Description
Technical field
The present invention relates to the method that the siliceous and calcareous raw material of a kind of reactive silica prepares xonotlite type calcium silicate material, belong to the preparations and applicatio field of ceramic, energy-saving building material.
Background technology
Calcium silicate material makes heat-insulation material by siliceous raw material and calcareous raw material through operations such as batching, Hydrothermal Synthesis, press filtration, shaping, oven dry.Calcium silicate material mainly contains two kinds, and one is tobermorite type, and one is xonotlite type.Xonotlite type calcium silicate material has the features such as unit weight is little, intensity is high, thermal conductivity is little, high temperature resistant, corrosion-resistant because of it, can be applicable to the adiabatic heat-insulation field of the insulation of heat power equipment and pipeline, insulation and building, boats and ships and train.
The preparation method of xonotlite type calcium silicate heat-preserving thermal insulation material has static hydrothermal method and Dynamic Hydrothermal method.Gaosheng Wei etc. selects silicon dioxide aerosol to be that siliceous raw material prepares Calucium Silicate powder insulating heat insulating material, and adding ceramic fiber is fortifying fibre.Notification number is that the Chinese patent " processing method of manufacture xonotlite type calcium silicate heat-preserving thermal insulation material " of CN 101880150A selects quartz sand to be siliceous raw material, active hydrogen calcium oxide is calcareous raw material dynamic autoclaved technology calcium-silicate thermal insulation material, but needs to add glass fibre and cotton thread.Notification number is that CN1204678A Chinese patent " manufacture method of heat-insulating calcium silicate refractory materials " selects the quartz of non-crystalline silicon micro mist or crystalline state to be siliceous raw material, needs to add natural organic fiber (fiber crops, cotton or vegetation fiber) simultaneously.Notification number is the Chinese patent " manufacture method of heat-insulation material of porous calcium silicate " of CN86103427A, with zeolite, diatomite, wilkinite etc. for siliceous raw material, adds asbestos as strongthener simultaneously.
At present, the siliceous raw material preparing xonotlite type calcium silicate material, with the quartz sand of crystalline state or based on amorphous silicon ash, diatomite, because siliceous raw material purity is not high, is rich in impurity, is difficult to synthesis of high purity lightweight calcium silicate material.Also need in conventional hydrothermal synthetic calcium silicate lagging material process to add the organic fibres such as cotton, paper pulp, regenerated fiber or the inorganic fibre such as glass fibre, asbestos strongthener (i.e. fortifying fibre) improves product strength simultaneously, but the supporting materials such as fiber add inappropriate, disperse uneven in moulding process, have a strong impact on the quality of calcium silicate material.Also need in simultaneous reactions process to add mineralizer to strengthen the crystallinity of calcium silicate material.
Summary of the invention
In order to solve above-mentioned problems of the prior art, the object of this invention is to provide that a kind of purity is high, light weight, density are little, intensity is high, the preparation method of the xonotlite type calcium silicate material of good stability.
To achieve these goals, the present invention adopts following technical scheme: method one: a kind of preparation method of xonotlite type calcium silicate material, and the step comprised is as follows:
1) get reactive silica siliceous raw material and calcareous raw material carries out grinding respectively, obtain granularity and be 80 ~ 325 object reactive silica silicon powders and lime powder;
2) by step 1) reactive silica silicon powder and lime powder, by its SiO
2/ CaO mol ratio is 0.85 ~ 1.25 to prepare burden, and is placed in the mixer of band whipping appts, adds process water and stirs into homogeneous material; Wherein, industrial water consumption is 10 ~ 15 with the volume mass ratio of high reactivity silicon-dioxide powdery and lime powder mixture; Described homogeneous material is inserted in confined reaction device after directly processing, and reacting by heating generates synthetic product;
3) by step 2) synthetic product after drying treatment, obtain described xonotlite type calcium silicate material through molding procedure.
Method two: a kind of preparation method of xonotlite type calcium silicate material, the step comprised is as follows:
1) get reactive silica siliceous raw material and calcareous raw material carries out grinding respectively, obtain granularity and be 80 ~ 325 object reactive silica silicon powders and lime powder;
2) by step 1) reactive silica silicon powder and lime powder, by its SiO
2/ CaO mol ratio is 0.85 ~ 1.25 to prepare burden, and is placed in the mixer of band whipping appts, adds process water and stirs into homogeneous material; Wherein, the add-on of process water is 10 ~ 15 with the volume mass ratio of reactive silica silicon powder and lime powder mixture; Described homogeneous material is inserted in confined reaction device after molding procedure, and reacting by heating generates synthetic product;
3) by step 2) synthetic product carry out drying treatment, obtain described xonotlite type calcium silicate material.
In two kinds of above-mentioned methods:
Step 1) SiO in active silica raw material used
2mass percentage be 80.0 ~ 98.0%, the titanium dioxide white residue after chrysotile fiber can be selected to carry magnesium, or/and serpentine tailing carries the titanium dioxide white residue after magnesium, is put forward magnesium mode and is adopted conventional pickling process and ammonium salt or acid salt roasting method to carry magnesium; In calcareous raw material, the mass percentage of CaO is 73 ~ 98.0%, can to select in the calcareous waste of unslaked lime, white lime or industrial oxidation at least a kind, and the calcareous waste of industrial oxidation is wherein in the calcinate of carbide slag or causticization white clay wantonly a kind;
Step 2) confined reaction device used is the band reactor of whipping appts or autoclave; Described Heating temperature is 180 ~ 225 DEG C, and temperature rise rate is 1.0 ~ 30.0 DEG C/min, and the reaction times is 2 ~ 16h;
Compression molding, the slurry flowing process of all available routine of above-mentioned molding procedure or copy to follow the example of and be shaped to section bar by processing requirement.
Above-mentioned drying treatment be the water ratio in its synthetic product is down to≤7.5%; Its drying mode can adopt any one mode of conventional drying.
Adopt the xonotlite type calcium silicate material that above-mentioned two kinds of different methods prepare, its performance index are: density≤140kg/m
3, thermal conductivity≤0.058W/ (m.K), linear shrinkage ratio≤1.8%, ultimate compression strength>=0.50Mpa, refractory temperature reaches 1000 DEG C.
The xonotlite type calcium silicate material adopting method of the present invention to prepare, its beneficial effect is as follows: the amorphous active silica raw material 1), namely chrysotile is or/and serpentine tailing carries titanium dioxide white residue after magnesium, there is high reactivity, be conducive to the carrying out of chemical reaction, such that hydrothermal temperature is lower, the reaction times is shorter.2) the siliceous raw material part selected by the present invention in threadiness, and contains vesicular structure, without the need to adding organic or inorganic reinforcing fiber in preparation process.3) Fe containing trace in this reaction siliceous raw material
3+can be used as mineralizer, without the need to adding mineralizer again in preparation process.4) it is high that the xonotlite type calcium silicate material that prepared by the present invention has intensity, the characteristics such as thermal conductivity is low, and chemical stability is good, and this xonotlite type calcium silicate material raw material availability is high, constant product quality; Can be applicable to the industries such as electric power, chemical industry, metallurgy, chemical industry, weaving, light industry building materials.5) characteristics such as the xonotlite type calcium silicate material lightweight prepared of the present invention, has heat insulating, fire prevention, fire-resistant and sound-absorbing sound insulation, containing asbestos, nontoxicity, security is high, is of value to and applies.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of xonotlite type calcium silicate material prepared by example 1.
Fig. 2 is the microscopic appearance image of xonotlite type calcium silicate material prepared by example 1.
Fig. 3 is the X ray diffracting spectrum of xonotlite type calcium silicate material prepared by example 2.
Fig. 4 is the microscopic appearance image of xonotlite type calcium silicate material prepared by example 2.
Fig. 5 is the X ray diffracting spectrum of xonotlite type calcium silicate material prepared by example 3.
Fig. 6 is the microscopic appearance image of xonotlite type calcium silicate material prepared by example 3.
Fig. 7 is the X ray diffracting spectrum of xonotlite type calcium silicate material prepared by example 4.
Fig. 8 is the microscopic appearance image of xonotlite type calcium silicate material prepared by example 4.
Fig. 9 is the exterior appearance image of xonotlite type calcium silicate material prepared by example 1.
Figure 10 is the exterior appearance image of xonotlite type calcium silicate material prepared by example 3.
Embodiment
Below in conjunction with example and accompanying drawing, technical scheme of the present invention is described in further detail.
Example 1
The raw material selected in example of the present invention is titanium dioxide white residue after chrysotile Carboxymethylcellulose lixiviate magnesium and unslaked lime.
1) by dioxide-containing silica be 98.0% chrysotile Carboxymethylcellulose lixiviate magnesium after titanium dioxide white residue and CaO content be 90.0% unslaked lime carry out grinding respectively, obtain fineness be 100 object reactive silica silicon powders and lime powder;
2) by step 1) levigate reactive silica silicon powder and lime powder, according to chemical composition analysis result, by SiO
2/ CaO mol ratio 0.90 is prepared burden, and be placed in the mixer of band whipping appts, after stirring than adding water for 12:1 by process water and high reactivity silicon-dioxide powdery and lime powder mixture volume mass, insert band whipping appts closed reactor under 180 DEG C of hydrothermal temperatures and 3.0MPa pressure condition hydro-thermal insulation 16h, obtain synthetic product, this synthetic product is xonotlite moulding mixture slurry;
3) by step 2) after hydro-thermal reaction after the cooling of xonotlite moulding mixture slurry, use conventional compression molding, under 0.3Mpa pressure, suppress dehydration forming with roller machine; Ordinary method is dry, obtains xonotlite type calcium silicate material, wherein quality water ratio 7.48%, density 117.91kg/m
3, thermal conductivity 0.047W/ (m.K), linear shrinkage ratio 0.15%, ultimate compression strength 0.80Mpa, refractory temperature reaches 1000 DEG C.
The X ray diffracting spectrum of xonotlite type calcium silicate material, microscopic appearance image, exterior appearance image as shown in Figure 1, Figure 2, shown in Fig. 9.As shown in Figure 1, the principal crystalline phase of the calcium silicate material of preparation is xonotlite, and characteristic diffraction peak peak type is sharp-pointed, good crystallinity; React perfect; Without other impurity components.From Fig. 2 and Fig. 9, the xonotlite type calcium silicate material outward appearance gray of preparation, microscopic appearance, in " ball algae shape ", is be made up of needle-like xonotlite whisker.
Example 2
The raw material selected in example of the present invention is that the titanium dioxide white residue after magnesium and white lime are carried in chrysotile fiber and acid salt or ammonium salt roasting; Its preparation method is substantially identical with example 1, is not repeating at this.
Its difference is:
1) by dioxide-containing silica be 94.3% chrysotile fiber and acid salt or ammonium salt roasting carry the titanium dioxide white residue after magnesium and CaO content be 73.0% white lime carry out grinding respectively, obtaining fineness is 80 object reactive silica silicon powders and white lime powder;
2) by step 1) levigate reactive silica silicon powder and white lime powder, according to chemical composition analysis result, by SiO
2/ CaO mol ratio 1.25 is prepared burden, and be placed in the mixer of band whipping appts, stir than for 11:1 adds water by process water and high reactivity silicon-dioxide powdery and lime powder mixture volume mass, hydro-thermal insulation 2h under 225 DEG C of hydrothermal temperatures and 1.5MPa pressure condition is inserted in autoclave after the compression molding process of routine, obtain synthetic product, this synthetic product is xonotlite type Calucium Silicate powder section bar;
3) by step 2) after the xonotlite type Calucium Silicate powder section bar cooling that obtains after hydro-thermal reaction, ordinary method is dry, obtains xonotlite type calcium silicate material, wherein quality water ratio 1.56%, density 96.57kg/m
3, thermal conductivity 0.041W/ (m.K), linear shrinkage ratio 0.06%, ultimate compression strength 0.76Mpa, refractory temperature reaches 1000 DEG C.
The X ray diffracting spectrum of xonotlite type calcium silicate material, microscopic appearance and exterior appearance image are as shown in Fig. 3, Fig. 4, Fig. 9.As shown in Figure 3, the calcium silicate material principal crystalline phase of preparation is xonotlite, and principal crystalline phase peak type is sharp-pointed, and good crystallinity, purity is higher, without other impurity components.From Fig. 4 and Fig. 9, the xonotlite type calcium silicate material outward appearance grey of preparation, microcosmic is still " ball algae shape " offspring, and " ball algae shape " particle is made up of the xonotlite whisker of needle-like.
Example 3
The raw material selected in example of the present invention is that serpentine tailing acidleach carries the titanium dioxide white residue after magnesium and causticization white clay through the calcining powder of 1000 DEG C; Its preparation method is substantially the same manner as Example 1, is not repeating at this.
Its difference is:
1) by dioxide-containing silica be 89.7% serpentine tailing acidleach carry magnesium after titanium dioxide white residue and CaO content be 90.0% the causticization burning of lime sludge products through 1000 DEG C of calcinings carry out grinding respectively, obtain 200 object reactive silica silicon powders and lime powder;
2) by step 1) levigate high reactivity silicon-dioxide powdery and lime powder, according to chemical composition analysis result, by SiO
2/ CaO mol ratio 0.85 is prepared burden, and be placed in the mixer of band whipping appts, after stirring than adding water for 15:1 by process water and high reactivity silicon-dioxide powdery and lime powder mixture volume mass, insert band whipping appts closed reactor under 190 DEG C of hydrothermal temperatures and 2.5MPa pressure condition hydro-thermal insulation 12h, the synthetic product obtained be xonotlite moulding mixture slurry;
3) by step 2) after xonotlite moulding mixture slurry cooling after hydro-thermal reaction, use slurry flowing process dehydration forming, obtain xonotlite type calcium silicate material after ordinary method drying, wherein quality water ratio 7.35%, density 94.44kg/m
3, thermal conductivity 0.041W/ (m.K), linear shrinkage ratio 0.07%, ultimate compression strength 0.69Mpa, refractory temperature reaches 1000 DEG C.
The X ray diffracting spectrum of xonotlite type calcium silicate material sample, microscopic appearance image and exterior appearance image are as shown in Fig. 5, Fig. 6 and Figure 10.As shown in Figure 5, the calcium silicate material of preparation is xonotlite crystal formation, and purity is higher.From Fig. 6 and Figure 10, the xonotlite type calcium silicate material outward appearance grey of preparation, microcosmic is still " ball algae shape " offspring, and " ball algae shape " particle is made up of the xonotlite whisker of needle-like.
Example 4
The raw material selected in example of the present invention is that the titanium dioxide white residue after magnesium and unslaked lime are carried in serpentine tailing and acid salt or ammonium salt roasting; Its preparation method is substantially the same manner as Example 1, is not repeating at this.
Its difference is:
1) by dioxide-containing silica be 80.0% serpentine tailing acid salt or ammonium salt roasting carry the titanium dioxide white residue after magnesium and CaO content be 98.0% unslaked lime carry out ball milling respectively, obtain 160 object reactive silica silicon powders and lime powder;
2) by step 1) levigate high reactivity silicon-dioxide powdery and lime powder, according to chemical composition analysis result, by SiO
2/ CaO mol ratio 1.0 is prepared burden, and be placed in the mixer of band whipping appts, after stirring than adding water for 10:1 by process water and high reactivity silicon-dioxide powdery and lime powder mixture volume mass, insert in the closed reactor of device to be mixed, hydro-thermal reaction 8h under 200 DEG C of hydrothermal temperatures and 2.4MPa pressure condition, obtaining synthetic product is xonotlite moulding mixture slurry;
3) by step 2) after xonotlite moulding mixture slurry cooling after hydro-thermal reaction, follow the example of dehydration forming with copying; Xonotlite type calcium silicate material is obtained, wherein quality water ratio 0.97%, density 118.74kg/m after dry
3, thermal conductivity 0.051W/ (m.K), linear shrinkage ratio 0.10%, ultimate compression strength 0.59Mpa, refractory temperature reaches 1000 DEG C.
The X ray diffracting spectrum of xonotlite type calcium silicate material sample, microscopic appearance image and appearance images are as shown in Fig. 7, Fig. 8 and Figure 10.Its calcium silicate material principal crystalline phase prepared is xonotlite, and principal crystalline phase peak type is sharp-pointed, and purity is higher.The xonotlite type calcium silicate material outward appearance of preparation is still grey, and microcosmic is " ball algae shape " offspring, and " ball algae shape " particle is made up of the xonotlite whisker of needle-like.
Example 5
The raw material selected in example of the present invention is the mixture through 1000 DEG C of causticization white claies calcined and carbide slag of titanium dioxide white residue after magnesium is carried in serpentine tailing and acid salt or ammonium salt roasting and mass ratio 1:1; Its preparation method is substantially identical with example 1, is not repeating at this.
Its difference is:
1) by dioxide-containing silica be the serpentine tailing acid salt of the 84.60% or titanium dioxide white residue after magnesium is carried in ammonium salt roasting and CaO content is 92.3%, the causticization white claies through 1000 DEG C of calcinings of mass ratio 1:1 and the mixture of carbide slag, carry out ball milling, obtain 325 object reactive silica silicon powders and lime powder;
2) by step 1) levigate reactive silica silicon powder and lime powder, according to chemical composition analysis result, by SiO
2/ CaO mol ratio 1.10 is prepared burden, and be placed in the mixer of band whipping appts, be that 12:1 adds water and stirs by process water and high reactivity silicon-dioxide powdery and lime powder mixture mass ratio, after conventional slurry flowing process forming processes, to insert in airtight autoclave hydro-thermal reaction 8h under 210 DEG C of hydrothermal temperatures and 2.0MPa pressure condition, obtaining synthetic product is xonotlite type Calucium Silicate powder section bar;
3) by step 2) after the xonotlite type Calucium Silicate powder section bar cooling that obtains after hydro-thermal reaction, ordinary method is dry, obtains xonotlite type calcium silicate material, wherein quality water ratio 5.46%, density 111.43kg/m
3, thermal conductivity 0.043W/ (m.K), linear shrinkage ratio 0.13%, ultimate compression strength 0.57Mpa, refractory temperature reaches 1000 DEG C.
The X ray diffracting spectrum of xonotlite type calcium silicate material sample, microscopic appearance image core exterior appearance are similar in appearance to Fig. 5, Fig. 6 and Fig. 9.Its calcium silicate material principal crystalline phase prepared is xonotlite, and characteristic diffraction peak intensity is higher, and purity is higher.The xonotlite type Calucium Silicate powder outward appearance grey of preparation, microcosmic is " ball algae shape " offspring, and " ball algae shape " particle is made up of the xonotlite whisker of needle-like.
Claims (8)
1. a preparation method for xonotlite type calcium silicate material, the step comprised is as follows:
1) get reactive silica siliceous raw material and calcareous raw material carries out grinding respectively, obtain granularity and be 80 ~ 325 object reactive silica silicon powders and lime powder;
2) by step 1) reactive silica silicon powder and lime powder, by its SiO
2/ CaO mol ratio is 0.85 ~ 1.25 to prepare burden, and is placed in the mixer of band whipping appts, adds process water and stirs into homogeneous material; Wherein, industrial water consumption is 10 ~ 15 with the volume mass ratio of high reactivity silicon-dioxide powdery and lime powder mixture; Described homogeneous material is inserted in confined reaction device after directly processing, and reacting by heating generates synthetic product;
3) by step 2) synthetic product after drying treatment, obtain described xonotlite type calcium silicate material through molding procedure.
2. a preparation method for xonotlite type calcium silicate material, the step comprised is as follows:
1) get reactive silica siliceous raw material and calcareous raw material carries out grinding respectively, obtain granularity and be 80 ~ 325 object reactive silica silicon powders and lime powder;
2) by step 1) reactive silica silicon powder and lime powder, by its SiO
2/ CaO mol ratio is 0.85 ~ 1.25 to prepare burden, and is placed in the mixer of band whipping appts, adds process water and stirs into homogeneous material; Wherein, the add-on of process water is 10 ~ 15 with the volume mass ratio of reactive silica silicon powder and lime powder mixture; Described homogeneous material is inserted in confined reaction device after forming processes, and reacting by heating generates synthetic product;
3) by step 2) synthetic product carry out drying treatment, obtain described xonotlite type calcium silicate material.
3. preparation method according to claim 1 and 2, is characterized in that: step 1) SiO in described active silica raw material
2mass percentage be 80.0 ~ 98.0%; In described calcareous raw material, the mass percentage of CaO is 73 ~ 98.0%.
4. preparation method according to claim 3, is characterized in that: described reactive silica siliceous raw material is at least one in the titanium dioxide white residue after titanium dioxide white residue after magnesium carried by chrysotile fiber or serpentine tailing carry magnesium; Described calcareous raw material is in the calcareous waste of unslaked lime, white lime or industrial oxidation at least a kind.
5. preparation method according to claim 4, is characterized in that: the calcareous waste of described industrial oxidation is in the calcinate of carbide slag or causticization white clay wantonly a kind.
6. preparation method according to claim 5, is characterized in that: step 2) described in confined reaction device be the band reactor of whipping appts or autoclave; Described Heating temperature is 180 ~ 225 DEG C, and temperature rise rate is 1.0 ~ 30.0 DEG C/min, and the reaction times is 2 ~ 16h.
7. preparation method according to claim 6, is characterized in that: step 3) described drying treatment be the water ratio of described synthetic product is down to≤7.5%.
8. preparation method according to claim 7, is characterized in that: the density≤140kg/m of described xonotlite type calcium silicate material
3, thermal conductivity≤0.058W/ (mK), linear shrinkage ratio≤1.8%, ultimate compression strength>=0.50Mpa, refractory temperature reaches 1000 DEG C.
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| CN109650941A (en) * | 2018-12-28 | 2019-04-19 | 蒙娜丽莎集团股份有限公司 | A kind of ceramic thin plate with humidity conditioning function synthesized with ceramic polished waste material low temperature |
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| CN105130360A (en) * | 2015-06-30 | 2015-12-09 | 武汉工程大学 | Lightweight calcium silicate plate prepared by using phosphate tailings and phosphorus slag as main materials |
| CN105130360B (en) * | 2015-06-30 | 2017-06-13 | 武汉工程大学 | A kind of utilization phosphorus mine tailing and phosphorus slag are light calcium silicate plate prepared by primary raw material |
| CN107857275A (en) * | 2017-03-15 | 2018-03-30 | 吉林大学 | The preparation method of xonotlite fiber material and obtained xonotlite fiber material |
| CN110885223A (en) * | 2018-09-07 | 2020-03-17 | 中国科学院过程工程研究所 | Calcium silicate powder, preparation method thereof, fireproof plate using calcium silicate powder and preparation method of fireproof plate |
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| CN110467368B (en) * | 2019-09-11 | 2021-11-26 | 上海海顾新材料科技有限公司 | Active excitant for inorganic solid waste building material and preparation method thereof |
| CN116175715A (en) * | 2023-02-23 | 2023-05-30 | 千年舟新材科技集团股份有限公司 | Anti-loss composite inorganic flame retardant, flame-retardant shaving board using same and manufacturing method thereof |
| CN116175715B (en) * | 2023-02-23 | 2023-11-03 | 千年舟新材科技集团股份有限公司 | Anti-loss composite inorganic flame retardant, flame-retardant shaving board using same and manufacturing method thereof |
| CN116063055A (en) * | 2023-03-22 | 2023-05-05 | 山东奥科金属制品集团有限公司 | Light calcium silicate board |
| CN116063055B (en) * | 2023-03-22 | 2023-08-18 | 山东奥科金属制品集团有限公司 | Light calcium silicate board |
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