CN108262003A - A kind of preparation method of diatom base hydration calcium silicate powder humidity adjusting material - Google Patents
A kind of preparation method of diatom base hydration calcium silicate powder humidity adjusting material Download PDFInfo
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- CN108262003A CN108262003A CN201710000914.1A CN201710000914A CN108262003A CN 108262003 A CN108262003 A CN 108262003A CN 201710000914 A CN201710000914 A CN 201710000914A CN 108262003 A CN108262003 A CN 108262003A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/14—Diatomaceous earth
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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Abstract
The present invention relates to inorganic functional powder field, specially a kind of preparation method of diatom base hydration calcium silicate powder humidity adjusting material.Using diatomite as natural mineral raw, make it that combination reaction occur with calcareous raw material and water in high temperature saturated steam, formed with hydrated calcium silicate powder humidity adjusting material as main component.Its key technology step includes：(1) by diatomite and calcareous raw material, dispensing mixing, the mixing water of addition siccative quality 20%~50% simultaneously continue to mix to substantially uniformity by a certain percentage；(2) reaction mixture carries out hydro-thermal reaction in 120~240 DEG C of saturated steam environment, and the time 2~for 24 hours；(3) it is moderately ground after the drying of gained sample, obtains diatom base hydration calcium silicate powder humidity adjusting material.Method provided by the present invention can obtain with hydrated calcium silicate powder body material as main component, can retain the abundant meso-hole structure of diatomite to a certain extent, and so as to assign the powder body material considerable moisture adsorption and releasing ability, humidity is excellent.
Description
Technical field
The present invention relates to inorganic functional powder field, specially a kind of system of diatom base hydration calcium silicate powder humidity adjusting material
Preparation Method.
Background technology
Generally use air-conditioning equipment makes residence environment keep comfortable temperature humidity in the production and living of people, but exists and set
The shortcomings of standby investment is high, energy consumption is big is also easy to cause indoor air quality issues in addition, influences the physical and mental health of people.
Humidity adjusting material refer to can according to the moisture absorption of itself/moisture releasing performance, residing for sensing in space Air Temperature/humidity change
Change, can automatically adjust the material of relative air humidity without consuming artificial energy source, the living environment of people can not only be improved,
Improve the preservation quality of article, it is often more important that reducing energy consumption, ecological environment being kept also to have profound significance.Generally recognize
It is, aperture in the tiny hole of 2~50nm, the influence for the moisture adsorption and releasing capacity of humidity adjusting material is the most notable.
As the important component in cement concrete, hydrated calcium silicate (Calcium silicate hydrate,
CSH) there is intrinsic microcellular structure (aperture d<2nm, in crystals)；In addition, with the difference of formation condition, in CSH crystalline substances
Also there are mesoporous (2~50nm of aperture) and macropore (more than aperture 50nm) to some extent between grain.Theoretically, with aquation silicon
Sour calcium building material as main component should have considerable moisture adsorption and releasing ability, but the building materials system such as cement concrete actually used
Product but fail to show expected humidity.Although it to find out its cause, is primarily due to micro- in the building materials such as cement concrete
Pore structure is enriched, but mesoporous, macropore content is relatively low, and is not connected each other between Kong Yukong, leads to hydrone inside product
Migration/diffusion it is difficult, can not realize reversible adsorption/desorption of a large amount of vapor, it is excellent cannot also to obtain humidity
Building material.
Invention content
In order to improve the humidity of hydrated calcium silicate CSH, the purpose of the present invention is to provide a kind of diatom base aquation silicon
The preparation method of sour calcium powder body humidity adjusting material, introduces more mesoporous and macropores in hydrated calcium silicate CSH, and mesoporous increase helps
In raising product to the reversible adsorption capacity of vapor, and macroporous structure can then provide the express passway of hydrone discrepancy, change
The environmental response speed of kind humidity adjusting material.
The technical scheme is that：
A kind of preparation method of diatom base hydration calcium silicate powder humidity adjusting material, includes the following steps：
(1) by diatomite and calcareous raw material dispensing mixing in proportion, calcareous raw material and diatomaceous ratio are with calcium silicon mole
Than counting between 0.45~0.99, adding in the mixing water of siccative quality 20%~50% and continuing to mix to substantially uniformity；
(2) reaction mixture carries out hydro-thermal reaction in 120~240 DEG C of saturated steam environment, and the time 2~for 24 hours；
(3) after the drying of gained sample, grinding obtains diatom base hydration calcium silicate powder humidity adjusting material.
The preparation method of the diatom base hydration calcium silicate powder humidity adjusting material, uses diatomite as siliceous raw material, silicon
SiO in diatomaceous earth2Quality than percentage composition not less than 60%, specific surface area is not less than 20m2/g。
The preparation method of the diatom base hydration calcium silicate powder humidity adjusting material, the main component of calcareous raw material is oxidation
Calcium CaO, calcium hydroxide Ca (OH)2Or both mixture.
The preparation method of the diatom base hydration calcium silicate powder humidity adjusting material, diatom base hydration calcium silicate powder damping
The main mineral constituent of material is hemicrystalline hydrated calcium silicate CSH (B), and the mesoporous content of 2~50nm sizes is not less than
0.06cm3/g。
Advantages of the present invention and advantageous effect are：
(1) preparation method provided by the present invention can obtain the aquation silicon of meso-hole structure prosperity by raw material of diatomite
Sour calcium powder body, hydrated product largely retain the pore property of diatomite material, so as to draw in hydrated calcium silicate
Enter more holes and be particularly the mesoporous of 3~50nm, be conducive to the raising of hydrated calcium silicate moisture adsorption and releasing ability.
(2) preparation method provided by the present invention is using diatomite as siliceous raw material, to diatomaceous purity, specific surface
Product etc. is of less demanding, can be translated into after hydro-thermal reaction with notable humidity and the production of the building materials of higher economic value
Product.Therefore, diatomite resource can be rationally utilized, improves diatomaceous economic value, is conducive to the natural ore deposit of middle-low grade diatomite
The utilization of Tibetan also have some reference value to the research and development of functional form construction material.
(3) technical advantage of preparation method provided by the present invention includes：Raw material is cheap and easy to get；Preparation method is easy to operate,
Production efficiency is high；Product moisture adsorption and releasing ability is strong；Diatomite resource can be rationally utilized, improves diatomaceous economic value.
Description of the drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of diatom base hydration calcium silicate powder obtained by different ratios of raw materials.It is horizontal in figure
2 θ of coordinate is the angle of diffraction (°), and ordinate Intensity is intensity (a.u.).
Fig. 2-Fig. 3 is the microstructure of diatom base hydration calcium silicate powder obtained by different hydration reaction temperature；Wherein, Fig. 2
For scanning electron microscope (SEM) photo, 120 DEG C of (a), 160 DEG C of (b), 200 DEG C of (c), 240 DEG C of (d)；Fig. 3 is special for pore-size distribution
It levies (BET method), abscissa Pore width are pore width (nm), and ordinate Pore surface area are hole specific surface
Product (m2·g-1).The control of calcium silicon mol ratio is 0.59 in reaction raw materials, the hydro-thermal reaction time 4h.
Fig. 4-Fig. 5 is the microstructure of diatom base hydration calcium silicate powder obtained by different hydration reaction times；Wherein, Fig. 4
For scanning electron microscope (SEM) photo, (a) 2h, (b) 4h, (c) 6h, (d) 8h；Fig. 5 is pore-size distribution feature (BET method), horizontal
Coordinate Pore width are pore width (nm), and ordinate Pore surface area are hole specific surface area (m2·g-1).Instead
It is 0.59 to answer calcium silicon mol ratio control in raw material, and hydrothermal temperature is 200 DEG C.
Fig. 6 (a)-Fig. 6 (b) is the moisture adsorption and releasing ability of gained diatom base hydration calcium silicate powder under different hydrothermal reaction conditions
With the comformity relation of mesoporous content；Wherein, 4h is reacted under (a) different temperatures, abscissa T is temperature (DEG C), ordinate (left side)
Moisture desorption rate are moisture releasing rate (%), and ordinate (right side) Pore volume (3~50nm) are hole specific volume
Product (cm3·g-1)；(b) different time is reacted under the conditions of 200 DEG C, abscissa T is temperature (DEG C), ordinate (left side) Moisture
Desorption rate are moisture releasing rate (%), and ordinate (right side) Pore volume (3~50nm) are hole specific volume (cm3·g-1)。
Specific embodiment
In specific implementation process, the present invention be enriched using pore structure, rule, orderly diatomite as natural material, make
Combination reaction occurs with calcareous raw material and water in high temperature saturated steam in it, is formed with hydrated calcium silicate powder as main component
Body humidity adjusting material, the powder body material can retain diatomaceous meso-hole structure feature to a certain extent, so as to assign the powder material
Expect considerable moisture adsorption and releasing ability, humidity is excellent.This method specifically includes following steps：
(1) by diatomite and calcareous raw material dispensing mixing by a certain percentage, the mix of siccative quality 20%~50% is added in
With water and continue to mix to substantially uniformity；
(2) reaction mixture carries out hydro-thermal reaction in 120~240 DEG C of saturated steam environment, and the time 2~for 24 hours；
(3) it is moderately ground after the drying of gained sample, obtains diatom base hydration calcium silicate powder humidity adjusting material.
Wherein, using diatomite as siliceous natural material, SiO in diatomite2Quality than percentage composition not less than 60% (excellent
It is selected as 70%~90%), specific surface area is not less than 20m2/ g (preferably 50~100m2/g).Used calcareous raw material is to aoxidize
Calcium CaO, calcium hydroxide Ca (OH)2Or both mixture, use calcareous raw material and diatomaceous ratio in raw mixture
With molar ratio computing between 0.45~0.99.The main mineral constituent of the hydration calcium silicate powder material is hemicrystalline aquation
Calcium silicates CSH (B), and the mesoporous content of 2~50nm sizes is not less than 0.06cm3/ g (preferably 0.10~0.30cm3/g)。
The present invention is further illustrated with reference to embodiments, but invention content is not limited to the embodiment：
Embodiment 1
In the present embodiment, Changbai production diatomite, SiO2Content is by percentage to the quality 61.38%, specific surface area
65m2/g.Using this diatomite as raw material, the detailed process of diatom base hydration calcium silicate powder humidity adjusting material is with technological parameter：
(1) diatomite and calcium hydroxide are added in into the mix of siccative quality 20% by 0.45 dispensing mixing of calcium silicon mol ratio
With water and continue to mix to substantially uniformity；
(2) reaction mixture carries out hydro-thermal reaction 4h in 200 DEG C of saturated steam environment；
(3) it is moderately ground after the drying of gained sample, obtains diatom base hydration calcium silicate powder humidity adjusting material.
X-ray diffraction (XRD) the result is shown in Figure 1 of hydration calcium silicate powder obtained by hydro-thermal reaction, analysis shows, in the powder
Reaction product is mainly hemicrystalline hydrated calcium silicate CSH (B).
Humidity detection shows that powder drying (105 DEG C) is placed on the hygroscopic capacity for 24 hours in 75% environment of relative humidity
Reach 8.32% (mass percent), then the amount of moisture releasing for 24 hours being transferred in 33% environment of relative humidity is then 2.87%, suction/moisture releasing
Ability is good.
Embodiment 2
In the present embodiment, diatom base hydration calcium silicate powder humidity adjusting material is made by each step of embodiment 1, the difference is that
In step (1) calcium oxide is used as calcareous raw material, and calcium silicon mol ratio is adjusted to 1.0；Other operating procedures are identical with condition.Water
X-ray diffraction (XRD) the result is shown in Figure 1 of hydration calcium silicate powder obtained by thermal response, analysis shows, reaction product master in the powder
To be hemicrystalline hydrated calcium silicate CSH (B), but have calcium hydroxide diffraction maximum remaining, show that calcium oxide is excessive in raw material.Damping
Performance detection shows that the hygroscopic capacity for 24 hours that powder drying (105 DEG C) is placed in 75% environment of relative humidity reaches 6.56%
(mass percent), then the amount of moisture releasing for 24 hours being transferred in 33% environment of relative humidity are then 2.11%, and suction/moisture releasing ability is preferable.
Embodiment 3
In the present embodiment, diatom base hydration calcium silicate powder humidity adjusting material is made by each step of embodiment 1, the difference is that
Hydrothermal reaction condition is adjusted to 120 DEG C, 4h in step (2)；Other operating procedures are identical with condition.Aquation silicon obtained by hydro-thermal reaction
Scanning electron microscope (SEM) microscopic appearance of sour calcium powder body is shown in Fig. 2 (a), shows the hydrated product hydrated calcium silicate very poor for crystallinity,
And reaction is incomplete.N2 adsorption experiment shows that the hydration calcium silicate powder reaches in the voids content of 2~50nm pore diameter ranges
0.012cm3/ g, humidity detection show that powder drying (105 DEG C) is placed on the suction for 24 hours in 75% environment of relative humidity
Moisture reaches 5.31% (mass percent), then the amount of moisture releasing for 24 hours being transferred in 33% environment of relative humidity is then 1.15%, is inhaled/
Moisture releasing ability is general.
Embodiment 4
In the present embodiment, diatom base hydration calcium silicate powder humidity adjusting material is made by each step of embodiment 3, the difference is that
In step (2) hydrothermal reaction condition be adjusted to 120 DEG C, for 24 hours；Other operating procedures are identical with condition.Humidity detection shows
The hygroscopic capacity for 24 hours that powder drying (105 DEG C) is placed in 75% environment of relative humidity reaches 8.45% (mass percent), then
The amount of moisture releasing for 24 hours being transferred in 33% environment of relative humidity is then 3.23%, and suction/moisture releasing ability is good.
Embodiment 5
In the present embodiment, diatom base hydration calcium silicate powder humidity adjusting material is made by each step of embodiment 1, the difference is that
Raw material proportioning is calculated as 0.83 with calcium silicon mol ratio in step (1)；Other operating procedures are identical with condition.Aquation obtained by hydro-thermal reaction
Scanning electron microscope (SEM) microscopic appearance of calcium silicate powder is shown in Fig. 2 (b), and it is hemicrystalline hydrated calcium silicate CSH to show hydrated product
(B), fragment shape crystal accumulation is agglomerating.N2 adsorption experiment shows hole of the hydration calcium silicate powder in 2~50nm pore diameter ranges
Content reaches 0.114cm3/ g, hence it is evident that higher than powder sample obtained by other reaction temperatures, same reaction time, see Fig. 3.Adjustable wet
It can detect and show that the hygroscopic capacity for 24 hours that powder drying (105 DEG C) is placed in 75% environment of relative humidity reaches 8.76% (matter
Measure percentage), then the amount of moisture releasing for 24 hours being transferred in 33% environment of relative humidity is then 3.32%, suction/moisture releasing ability is good.
Embodiment 6
In the present embodiment, diatom base hydration calcium silicate powder humidity adjusting material is made by each step of embodiment 5, the difference is that
Hydrothermal reaction condition is adjusted to 240 DEG C, 4h in step (2)；Other operating procedures are identical with condition.Aquation silicon obtained by hydro-thermal reaction
Scanning electron microscope (SEM) microscopic appearance of sour calcium powder body is shown in Fig. 2 (c), and it is crystallinity hydrated calcium silicate Tuo Beimo to show hydrated product
Carry out stone, crystal accumulation is agglomerating.N2 adsorption experiment shows voids content of the hydration calcium silicate powder in 2~50nm pore diameter ranges
Reach 0.062cm3/g.Humidity detection shows that powder drying (105 DEG C) is placed in 75% environment of relative humidity
Hygroscopic capacity reaches 4.93% (mass percent) for 24 hours, then the amount of moisture releasing for 24 hours being transferred in 33% environment of relative humidity is then
1.84%, suction/moisture releasing ability is good.
Embodiment 7
In the present embodiment, diatom base hydration calcium silicate powder humidity adjusting material is made by each step of embodiment 5, the difference is that
Hydrothermal reaction condition is adjusted to 200 DEG C, 2h in step (2)；Other operating procedures are identical with condition.Aquation silicon obtained by hydro-thermal reaction
Scanning electron microscope (SEM) microscopic appearance of sour calcium powder body is shown in Fig. 4 (a), and it is hemicrystalline hydrated calcium silicate CSH to show hydrated product
(B), but hydration reaction is incomplete.N2 adsorption experiment shows that the hydration calcium silicate powder contains in the hole of 2~50nm pore diameter ranges
Amount reaches 0.031cm3/ g, hence it is evident that higher than powder sample obtained by other reaction temperatures, same reaction time, see Fig. 5.Humidity
Detection shows that the hygroscopic capacity for 24 hours that powder drying (105 DEG C) is placed in 75% environment of relative humidity reaches 7.11% (quality
Percentage), then the amount of moisture releasing for 24 hours being transferred in 33% environment of relative humidity is then 1.57%, suction/moisture releasing ability is preferable.
Embodiment 8
In the present embodiment, Changbai production diatomite, SiO2Content is by percentage to the quality 85.61%, specific surface area
22m2/g.Using this diatomite as raw material, the detailed process of diatom base hydration calcium silicate powder humidity adjusting material is with technological parameter：
(1) diatomite and calcium hydroxide are added in into the mix of siccative quality 50% by 0.83 dispensing mixing of calcium silicon mol ratio
With water and continue to mix to substantially uniformity；
(2) reaction mixture carries out hydro-thermal reaction 4h in 200 DEG C of saturated steam environment；
(3) it is moderately ground after the drying of gained sample, obtains diatom base hydration calcium silicate powder humidity adjusting material
The detection of water humidity shows that powder drying (105 DEG C) is placed on the moisture absorption for 24 hours in 75% environment of relative humidity
Amount reaches 4.25% (mass percent), then the amount of moisture releasing for 24 hours being transferred in 33% environment of relative humidity is then 1.40%, inhales/puts
Wet ability is preferable.
As shown in Fig. 2 (a)-(d), it can be seen that instead from different hydration reaction temperature scanning electron microscope (SEM) photos
It is all in the case of 4h between seasonable, with the raising of hydrothermal temperature, reaction product is gradually changed by amorphous gelinite (Fig. 2 a)
It is converted again to crystalline solid (Fig. 2 c, 2d) for semi-crystalline (Fig. 2 b).Compare the moisture absorption and desorption property discovery of respective sample, lower temperature
Under obtained hydrated calcium silicate product CSH (B) the moisture adsorption and releasing ability of sample is improved advantageously.
As shown in figure 3, the pore structure analysis result that sample obtained by 4h is reacted under different temperatures can be seen that with reaction temperature
The raising of degree, the pore size distribution peak area first increases and then decreases of 3~20nm positions, the pore size distribution peak under the conditions of 200 DEG C in sample
Significantly.At the same time, test shows that suction/moisture releasing rate of respective sample is also maximum, i.e. diatom base hydration calcium silicate powder
Damping ability is directly related with the mesoporous content of sample.
As shown in Fig. 4 (a)-(d), it can be seen that instead from different hydration reaction time scanning electron microscope (SEM) photos
The temperature is answered to be all in the case of 200 DEG C, with the extension of hydro-thermal time, reaction product is gradually from semi-crystalline (Fig. 2 a) to crystalline solid
(Fig. 2 b, 2c, 2d) is converted；With the progress of hydro-thermal reaction, crystalline product size gradually increases, heap poly structure each other
It is more close.Moisture absorption and desorption property than respective sample finds that the hydro-thermal reaction time under 200 DEG C and higher temperature is unsuitable long,
Otherwise certain influence may be generated on the moisture adsorption and releasing ability of sample.
As shown in figure 5, the pore structure analysis result from sample obtained by the differential responses time at 200 DEG C can be seen that with anti-
Extension between seasonable, the pore size distribution peak area first increases and then decreases of 3~20nm positions, the pore size distribution peak under the conditions of 4h in sample
Significantly.At the same time, test shows that suction/moisture releasing rate of respective sample is also maximum, i.e. diatom base hydration calcium silicate powder
Damping ability is directly related with the mesoporous content of sample.
As shown in Fig. 6 (a), (b), the further analysis of diatom base hydrated calcium silicate damping powder structure-performance is calculated
Show that the moisture adsorption and releasing ability of diatom base hydrated calcium silicate is directly related with its mesoporous content, in hydrothermal temperature and time tune
The consistency of changing rule when whole is good.
Embodiment the result shows that, the present invention have notable humidity hydration calcium silicate powder preparation method, be with
Diatomite is natural siliceous raw material, is obtained using the hydro-thermal combination reaction of the calcareous raw materials such as diatomite and calcium oxide, calcium hydroxide
The hydrated calcium silicate that crystallinity is appropriate, meso-hole structure is abundant, can be shown when ambient humidity changes considerable water vapor adsorption/
Desorption is moisture adsorption and releasing ability.Method provided by the present invention can obtain with hydrated calcium silicate powder body material as main component, can be
Retain the abundant meso-hole structure of diatomite, so as to assign the powder body material considerable moisture adsorption and releasing ability, adjustable wet to a certain extent
It can be excellent.
Claims (4)
1. a kind of preparation method of diatom base hydration calcium silicate powder humidity adjusting material, which is characterized in that include the following steps：
(1) by diatomite and calcareous raw material dispensing mixing in proportion, calcareous raw material and diatomaceous ratio are in terms of calcium silicon mol ratio
Between 0.45~0.99, add in the mixing water of siccative quality 20%~50% and continue to mix to substantially uniformity；
(2) reaction mixture carries out hydro-thermal reaction in 120~240 DEG C of saturated steam environment, and the time 2~for 24 hours；
(3) after the drying of gained sample, grinding obtains diatom base hydration calcium silicate powder humidity adjusting material.
2. the preparation method of diatom base hydration calcium silicate powder humidity adjusting material according to claim 1, which is characterized in that adopt
It is siliceous raw material with diatomite, SiO in diatomite2Quality than percentage composition not less than 60%, specific surface area is not less than 20m2/
g。
3. the preparation method of diatom base hydration calcium silicate powder humidity adjusting material according to claim 1, which is characterized in that calcium
The main component of matter raw material is calcium oxide CaO, calcium hydroxide Ca (OH)2Or both mixture.
4. the preparation method of diatom base hydration calcium silicate powder humidity adjusting material according to claim 1, which is characterized in that silicon
The main mineral constituent of algae base hydration calcium silicate powder humidity adjusting material is hemicrystalline hydrated calcium silicate CSH (B), and 2~50nm
The mesoporous content of size is not less than 0.06cm3/g。
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| CN112716027A (en) * | 2021-03-04 | 2021-04-30 | 河南中烟工业有限责任公司 | Method for adjusting moisture content of case-packed tobacco flakes |
| CN112898041A (en) * | 2018-09-11 | 2021-06-04 | 淮阴工学院 | Application of attapulgite or bentonite-based plant fiber composite humidity control material in indoor air purification |
| US20210394154A1 (en) * | 2020-06-23 | 2021-12-23 | The United States Of America, As Represented By The Secretary Of Agriculture | Composition and method for reducing ammonia and soluble phosphorus in runoff and leaching from animal manure |
| CN113993372A (en) * | 2019-07-05 | 2022-01-28 | 太平洋水泥株式会社 | Material for cultivation and manufacturing method thereof |
| CN116425509A (en) * | 2023-04-11 | 2023-07-14 | 重庆大学 | Nanometer calcium silicate hydrate gel humidity-regulating material and preparation method thereof |
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