CN105439181A - Preparation method of high-dispersity nanocalcium hydroxide - Google Patents
Preparation method of high-dispersity nanocalcium hydroxide Download PDFInfo
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- CN105439181A CN105439181A CN201510994803.8A CN201510994803A CN105439181A CN 105439181 A CN105439181 A CN 105439181A CN 201510994803 A CN201510994803 A CN 201510994803A CN 105439181 A CN105439181 A CN 105439181A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/02—Oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- Organic Chemistry (AREA)
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- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of high-dispersity nanocalcium hydroxide. The preparation method comprises the following steps: (1) weighing materials; (2) carrying out ultrasonic pre-treatment; (3) preparing; (4) centrifuging and washing; and (5) drying and crushing. According to the preparation method of the high-dispersity nanocalcium hydroxide, provided by the invention, through a reasonable formula design and scientific technical conditions, prepared calcium hydroxide particles have uniform grain diameters, no block masses and stable quality, and can meet the requirements on the high-dispersity nanocalcium hydroxide of fields including industrial production and the like; and the preparation process is simple and has no dangers to the environment.
Description
Technical field
The present invention relates to calcium hydroxide preparing technical field, particularly relate to a kind of preparation method of high dispersancy nano calcium hydroxide.
Background technology
Calcium hydroxide has a wide range of applications in the industrial production such as rubber, cement, and it increases to some extent in environmental area application in recent years.As in solid waste burning, calcium hydroxide can be used as dechlorinating agent, sweetening agent etc.In improvement soil acidification and heavy metal contamination process, calcium hydroxide can be used as neutralization reagent or stablizer.The auxiliary agent etc. of environment-acceptable material is can be used as in plastics preparation process.
Nano material can produce special-effect because of its surface effects and volume effect etc., has special physicochemical property, thus becomes present material preparation field study hotspot.But the technical requirements of nano material preparation process is higher, careless slightly, nanoparticle again can be reunited and be grown up, and forms agglomerate, affects material property.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of preparation method of high-dispersion nano calcium hydroxide, can solve calcium hydroxide particle particle diameter inequality prepared by existing method, the problems such as the nano level calcium hydroxide quality instability of preparation.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: the preparation method providing a kind of high dispersancy nano calcium hydroxide, comprises the steps:
(1) material takes: take dispersion agent 25 ~ 40 parts, 45wt% calcium chloride solution 15 ~ 20 parts, 50wt% sodium hydroxide solution 18 ~ 22 parts, SDBS5 ~ 8 part;
(2) ultrasonic pretreatment: the dispersion agent taken in step (1) and SDBS are joined in calcium chloride solution, ultrasonic 4 ~ 5h;
(3) preparation feedback: in the solution that step (2) is obtained, slowly add the sodium hydroxide that step (1) takes under certain condition;
(4) centrifuge washing: centrifugal under the solution certain condition that step (3) is obtained, removing supernatant, precipitates 3 ~ 4 times by washed with de-ionized water;
(5) drying and crushing: the throw out vacuum-drying obtained by step (4), puts into pulverizer by dry for gained thing and pulverizes, be described high dispersancy nano calcium hydroxide.
In a preferred embodiment of the present invention, in described step (1), described dispersion agent is mass ratio is that the polyethylene of 1 ~ 3:2 ~ 5 is than the mixture coughing up ketone and polyoxyethylene glycol.
In a preferred embodiment of the present invention, in described step (3), described reaction conditions is constant temperature 35 ~ 45 DEG C, and adding sodium hydroxide solution speed is 3 ~ 4ml/min.
In a preferred embodiment of the present invention, in described step (4), described centrifugal condition is: first carry out once centrifugal, removes supernatant liquor, then carries out secondary centrifuging; Wherein, a described centrifugal condition is: centrifugal speed 500 ~ 700r/min, centrifugation time 20min; Described secondary centrifuging condition is: centrifugal speed 1500 ~ 1700r/min, centrifugation time 30min.
In a preferred embodiment of the present invention, in described step (5), described drying conditions is: vacuum tightness 0.10 ~ 0.20Mpa, temperature 70 ~ 90 DEG C, time of drying 4 ~ 5h.
In a preferred embodiment of the present invention, described calcium hydroxide particle granularity is 95 ~ 120nm.
The invention has the beneficial effects as follows: the preparation method of a kind of high-dispersion nano calcium hydroxide of the present invention, by rational formula design and the processing condition of science, make prepared calcium hydroxide particle uniform particle sizes, without agglomerate, steady quality, can meet the demand of the fields such as industrial production to high-purity hydrogen calcium oxide, and preparation technology is simple, to environment without harm.
Embodiment
Below preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
The embodiment of the present invention comprises:
Embodiment 1
(1) material takes: take in mass ratio for the polyethylene of 3:5 mixing is than the dispersion agent 40 parts coughing up ketone and polyoxyethylene glycol mixture, 45% calcium chloride solution 20 parts, 50% sodium hydroxide solution 22 parts, SDBS8 part;
(2) ultrasonic pretreatment: the dispersion agent taken in step (1) and SDBS are joined in calcium chloride solution, ultrasonic 5h;
(3) preparation feedback: in the solution that step (2) is obtained, constant temperature 45 DEG C, ultrasonic, slowly add with 4ml/min the sodium hydroxide solution that step (1) takes;
(4) centrifuge washing: by solution obtained for step (3) with the centrifugal 20min of the centrifugal speed of 700r/min, remove supernatant liquor, then with the centrifugal speed secondary centrifuging 30min of 1700r/min, removing supernatant liquor, precipitates 4 times by washed with de-ionized water;
(5) drying and crushing: by throw out obtained for step (4) at vacuum tightness 0.10 ~ 0.20Mpa, under temperature 90 DEG C of conditions, dry 5h, puts into pulverizer by dry for gained thing and pulverizes, be described high dispersancy nano calcium hydroxide.
Embodiment 2
(1) material takes: take in mass ratio for the polyethylene of 1:2 mixing is than the dispersion agent 25 parts coughing up ketone and polyoxyethylene glycol mixture, 45% calcium chloride solution 15 parts, 50% sodium hydroxide solution 18 parts, SDBS5 part;
(2) ultrasonic pretreatment: the dispersion agent taken in step (1) and SDBS are joined in calcium chloride solution, ultrasonic 4h;
(3) preparation feedback: in the solution that step (2) is obtained, constant temperature 35 DEG C, ultrasonic, slowly add with 3ml/min the sodium hydroxide solution that step (1) takes;
(4) centrifuge washing: the solution 500r/min centrifugal speed centrifugal 20min obtained by step (3), removes supernatant, 1500r/min secondary centrifuging 30min, and removing supernatant, precipitates 3 times by washed with de-ionized water;
(5) drying and crushing: by throw out obtained for step (4) at vacuum tightness 0.10 ~ 0.20Mpa, under temperature 70 C condition, dry 4h, puts into pulverizer by dry for gained thing and pulverizes, be described high dispersancy nano calcium hydroxide.
Calcium hydroxide particle granularity prepared by aforesaid method is 95 ~ 120nm.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (6)
1. a preparation method for high dispersancy nano calcium hydroxide, is characterized in that, comprises the steps:
(1) material takes: take dispersion agent 25 ~ 40 parts, 45wt% calcium chloride solution 15 ~ 20 parts, 50wt% sodium hydroxide solution 18 ~ 22 parts, SDBS5 ~ 8 part;
(2) ultrasonic pretreatment: the dispersion agent taken in step (1) and SDBS are joined in calcium chloride solution, ultrasonic 4 ~ 5h;
(3) preparation feedback: in the solution that step (2) is obtained, slowly add the sodium hydroxide that step (1) takes under certain condition;
(4) centrifuge washing: centrifugal under the solution certain condition that step (3) is obtained, removing supernatant, precipitates 3 ~ 4 times by washed with de-ionized water;
(5) drying and crushing: the throw out vacuum-drying obtained by step (4), puts into pulverizer by dry for gained thing and pulverizes, be described high dispersancy nano calcium hydroxide.
2. the preparation method of a kind of high dispersancy nano calcium hydroxide according to claim 1, is characterized in that, in described step (1), described dispersion agent is mass ratio is that the polyethylene of 1 ~ 3:2 ~ 5 is than the mixture coughing up ketone and polyoxyethylene glycol.
3. the preparation method of a kind of high dispersancy nano calcium hydroxide according to claim 1, is characterized in that, in described step (3), described reaction conditions is constant temperature 35 ~ 45 DEG C, and adding sodium hydroxide solution speed is 3 ~ 4ml/min.
4. the preparation method of a kind of high dispersancy nano calcium hydroxide according to claim 1, is characterized in that, in described step (4), described centrifugal condition is: first carry out once centrifugal, removes supernatant liquor, then carries out secondary centrifuging; Wherein, a described centrifugal condition is: centrifugal speed 500 ~ 700r/min, centrifugation time 20min; Described secondary centrifuging condition is: centrifugal speed 1500 ~ 1700r/min, centrifugation time 30min.
5. the preparation method of a kind of high dispersancy nano calcium hydroxide according to claim 1, is characterized in that, in described step (5), described drying conditions is: vacuum tightness 0.10 ~ 0.20Mpa, temperature 70 ~ 90 DEG C, time of drying 4 ~ 5h.
6. according to the preparation method of a kind of high dispersancy nano calcium hydroxide one of claim 1 to 5 Suo Shu, it is characterized in that, described calcium hydroxide particle granularity is 95 ~ 120nm.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107854322A (en) * | 2017-10-24 | 2018-03-30 | 武汉大学 | A kind of preparation method of nano calcium hydroxide for root canal filling material |
CN108689421A (en) * | 2017-11-06 | 2018-10-23 | 天水师范学院 | A kind of preparation method of dispersed nano calcium hydroxide |
CN108821613A (en) * | 2018-07-04 | 2018-11-16 | 衢州市远方化工厂(普通合伙) | A kind of preparation process of nanometer of anti-agglomeration calcium hydroxide slurry |
CN109261117A (en) * | 2018-08-08 | 2019-01-25 | 河南工程学院 | A kind of preparation method loading spherical nanometer calcium salt oxidizing agent based on rectorite |
CN114522638A (en) * | 2022-01-11 | 2022-05-24 | 山东师范大学 | Continuous production system and method for calcium hydroxide with controllable crystal morphology |
CN114853046A (en) * | 2022-05-26 | 2022-08-05 | 镇江华茂新材料科技有限公司 | Method for preparing nano calcium hydroxide by adopting micro-channel reactor |
-
2015
- 2015-12-28 CN CN201510994803.8A patent/CN105439181A/en active Pending
Non-Patent Citations (1)
Title |
---|
许兢: "纳米氢氧化钙的合成、表征及其在可环境消纳塑料中的应用", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107854322A (en) * | 2017-10-24 | 2018-03-30 | 武汉大学 | A kind of preparation method of nano calcium hydroxide for root canal filling material |
CN108689421A (en) * | 2017-11-06 | 2018-10-23 | 天水师范学院 | A kind of preparation method of dispersed nano calcium hydroxide |
CN108821613A (en) * | 2018-07-04 | 2018-11-16 | 衢州市远方化工厂(普通合伙) | A kind of preparation process of nanometer of anti-agglomeration calcium hydroxide slurry |
CN109261117A (en) * | 2018-08-08 | 2019-01-25 | 河南工程学院 | A kind of preparation method loading spherical nanometer calcium salt oxidizing agent based on rectorite |
CN109261117B (en) * | 2018-08-08 | 2021-06-22 | 河南工程学院 | Preparation method of rectorite-based spherical nano calcium salt loaded oxidant |
CN114522638A (en) * | 2022-01-11 | 2022-05-24 | 山东师范大学 | Continuous production system and method for calcium hydroxide with controllable crystal morphology |
CN114853046A (en) * | 2022-05-26 | 2022-08-05 | 镇江华茂新材料科技有限公司 | Method for preparing nano calcium hydroxide by adopting micro-channel reactor |
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