CN105561899A - Preparation method of high-surface-activity microcapsule calcium hydroxide - Google Patents
Preparation method of high-surface-activity microcapsule calcium hydroxide Download PDFInfo
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- CN105561899A CN105561899A CN201510994804.2A CN201510994804A CN105561899A CN 105561899 A CN105561899 A CN 105561899A CN 201510994804 A CN201510994804 A CN 201510994804A CN 105561899 A CN105561899 A CN 105561899A
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- calcium hydroxide
- preparation
- high surface
- microcapsules
- solution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- 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
Abstract
The invention discloses a preparation method of a high-surface-activity microcapsule calcium hydroxide, wherein the preparation method includes the following steps: (1) weighing materials; (2) preparing a capsule pre-polymer; (3) preparing high-purity calcium hydroxide; (4) performing centrifugal washing; and (5) preparing the microcapsule calcium hydroxide. According to the preparation method of the high-surface-activity microcapsule calcium hydroxide, through reasonable formula design and scientific technological conditions, the prepared calcium hydroxide microcapsule can be effectively avoided from undergoing a reaction with carbon dioxide in air, so as to solve the problems of low purity of calcium hydroxide, unstable quality and the like. In addition, the organic polymer covers the surface of the calcium hydroxide, so that the effect of surface modification is achieved, and a dispersion stability problem of calcium oxide particles in polymers can be improved.
Description
Technical field
The present invention relates to calcium hydroxide preparing technical field, particularly relate to a kind of preparation method of high surface microcapsules calcium hydroxide.
Background technology
Inorganic powder material is widely used in the traditional industries such as cement, coating, and in recent years, its application in the new industries such as Polymer materialspreparation also gets more and more, and in this type of industry to the purity of inorganic powder material and stability requirement higher.
Calcium hydroxide is widely used in the industrial production such as rubber, cement, and it increases to some extent in environmental area application in addition.In solid waste burning, calcium hydroxide can be used as antichlor, desulfurizing agent.In improvement soil acidification and heavy metal pollution process, calcium hydroxide can be used as neutralization reagent or stabilizing agent.The auxiliary agent etc. of environment-acceptable material is can be used as in plastics preparation process.But because calcium hydroxide powder is unstable, easily and Carbon Dioxide in Air reaction etc., greatly limit the commercial Application of calcium hydroxide inorganic particle.The effective ways of stable calcium hydroxide performance by inorganic particle capsulation.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of preparation method of high surface microcapsules calcium hydroxide, the calcium hydroxide powder that can solve preparation easily and Carbon Dioxide in Air react, cause purity not high, the problems such as quality is unstable, limit its commercial Application.
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 surface microcapsules calcium hydroxide, comprises the steps:
(1) material takes: take dispersant 25 ~ 40 parts, capsule preparations 35 ~ 40 parts, 45wt% calcium chloride solution 15 ~ 20 parts, 50wt% sodium hydroxide solution 18 ~ 22 parts, SDBS5 ~ 8 part;
(2) prepare capsule performed polymer: the capsule preparations taken in step (1) is put into there-necked flask, under certain condition, react 3 ~ 4h;
(3) High Purity Hydrogen calcium oxide is prepared: join in calcium chloride solution by the dispersant taken in step (1) and SDBS, ultrasonic 4 ~ 5h; In the solution that step (2) is obtained, under certain condition, slowly add the NaOH that step (1) takes;
(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) microcapsules calcium hydroxide is prepared: precipitation prepared by step (4) joined in prepolymer solution prepared by step (2), react 4 ~ 5h under certain condition, decompression dehydration, vacuum drying obtains end product.
In a preferred embodiment of the present invention, in described step (1), described dispersant to be mass ratio the be polyethylene of 1 ~ 3:2 ~ 5 is than the mixture coughing up ketone and polyethylene glycol, and described capsule preparations is mass ratio is the formaldehyde of 1 ~ 3:2 ~ 7 and the mixed liquor of phenol.
In a preferred embodiment of the present invention, in described step (2), described reaction condition is: temperature 60 ~ 75 DEG C, mixing speed 800 ~ 1000r/min.
In a preferred embodiment of the present invention, in described step (3), described reaction condition is constant temperature 35 ~ 45 DEG C, and the rate of addition of described sodium hydroxide solution 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, carries out secondary centrifuging after removing supernatant, wherein, and a centrifugal speed 500 ~ 700r/min, time 20min; Secondary centrifuging speed 1500 ~ 1700r/min, time 30min.
In a preferred embodiment of the present invention, in described step (5), described reaction condition is: with 4 ~ 6 DEG C/min temperature programming to 75 DEG C, stirs 4 ~ 5h, be cooled to room temperature with 1000 ~ 1500r/min mixing speed.
In a preferred embodiment of the present invention, in described step (5), described drying condition is: vacuum 0.10 ~ 0.20MPa, temperature 70 ~ 90 DEG C, drying time 6 ~ 7h.
The invention has the beneficial effects as follows: the preparation method of a kind of high surface microcapsules of the present invention calcium hydroxide, by rational formula design and the process conditions of science, prepared calcium hydroxide microcapsules be effectively prevent react with Carbon Dioxide in Air, cause calcium hydroxide purity not high, the problems such as quality is unstable, in addition organic polymer is covered calcium hydroxide surface, reach the effect of surface modification, calcium oxide particle stably dispersing sex chromosome mosaicism in the polymer can be improved.
Detailed description of the invention
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 dispersant 40 parts coughing up ketone and polyethylene glycol mixture, be the formaldehyde of 3:7 mixing and the capsule preparation 40 parts of phenol mixing sol by volume, 45wt% calcium chloride solution 20 parts, 50wt% sodium hydroxide solution 22 parts, SDBS8 part;
(2) prepare capsule performed polymer: the capsule preparations taken in step (1) is put into there-necked flask, 75 DEG C of constant temperature, stir with 1000r/min mixing speed, reaction 4h;
(3) High Purity Hydrogen calcium oxide is prepared: join in calcium chloride solution by the dispersant taken in step (1) and SDBS, ultrasonic 5h; 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: the solution 700r/min centrifugal speed centrifugal 20min obtained by step (3), removes supernatant, 1700r/min secondary centrifuging 30min, and removing supernatant, precipitates 4 times by washed with de-ionized water;
(5) microcapsules calcium hydroxide is prepared: precipitation prepared by step (4) joined in prepolymer solution prepared by step (2), 6 DEG C/min temperature programming to 75 DEG C, 5h is stirred with 1500r/min mixing speed, be cooled to room temperature, decompression dehydration, at 0.1 ~ 0.2MPa, under temperature 90 DEG C of conditions, dry 7h, obtains end product.
Embodiment 2
(1) material takes: take in mass ratio for the polyethylene of 1:2 mixing is than the dispersant 25 parts coughing up ketone and polyethylene glycol mixture, be the formaldehyde of 1:2 mixing and the capsule preparation 35 parts of phenol mixing sol by volume, 45wt% calcium chloride solution 15 parts, 50wt% sodium hydroxide solution 18 parts, SDBS5 part;
(2) prepare capsule performed polymer: the capsule preparations taken in step (1) is put into there-necked flask, 60 DEG C of constant temperature, stir with 800r/min mixing speed, reaction 3h;
(3) High Purity Hydrogen calcium oxide is prepared: join in calcium chloride solution by the dispersant taken in step (1) and SDBS, ultrasonic 4h; 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) microcapsules calcium hydroxide is prepared: precipitation prepared by step (4) joined in prepolymer solution prepared by step (2), 4 DEG C/min temperature programming to 75 DEG C, 4h is stirred with 1000r/min mixing speed, be cooled to room temperature, decompression dehydration, at 0.1 ~ 0.2Mpa, under temperature 70 C condition, dry 6h, obtains end product.
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 (7)
1. a preparation method for high surface microcapsules calcium hydroxide, is characterized in that, comprises the steps:
(1) material takes: take dispersant 25 ~ 40 parts, capsule preparations 35 ~ 40 parts, 45wt% calcium chloride solution 15 ~ 20 parts, 50wt% sodium hydroxide solution 18 ~ 22 parts, SDBS5 ~ 8 part;
(2) prepare capsule performed polymer: the capsule preparations taken in step (1) is put into there-necked flask, under certain condition, react 3 ~ 4h;
(3) High Purity Hydrogen calcium oxide is prepared: join in calcium chloride solution by the dispersant taken in step (1) and SDBS, ultrasonic 4 ~ 5h; In the solution that step (2) is obtained, under certain condition, slowly add the NaOH that step (1) takes;
(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) microcapsules calcium hydroxide is prepared: precipitation prepared by step (4) joined in prepolymer solution prepared by step (2), react 4 ~ 5h under certain condition, decompression dehydration, vacuum drying obtains end product.
2. the preparation method of a kind of high surface microcapsules calcium hydroxide according to claim 1, it is characterized in that, in described step (1), described dispersant to be mass ratio the be polyethylene of 1 ~ 3:2 ~ 5 is than the mixture coughing up ketone and polyethylene glycol, and described capsule preparations is mass ratio is the formaldehyde of 1 ~ 3:2 ~ 7 and the mixed liquor of phenol.
3. the preparation method of a kind of high surface microcapsules calcium hydroxide according to claim 1, it is characterized in that, in described step (2), described reaction condition is: temperature 60 ~ 75 DEG C, mixing speed 800 ~ 1000r/min.
4. the preparation method of a kind of high surface microcapsules calcium hydroxide according to claim 1, is characterized in that, in described step (3), described reaction condition is constant temperature 35 ~ 45 DEG C, and the rate of addition of described sodium hydroxide solution is 3 ~ 4ml/min.
5. the preparation method of a kind of high surface microcapsules calcium hydroxide according to claim 1, it is characterized in that, in described step (4), described centrifugal condition is: first carry out once centrifugal, secondary centrifuging is carried out after removing supernatant, wherein, a centrifugal speed 500 ~ 700r/min, time 20min; Secondary centrifuging speed 1500 ~ 1700r/min, time 30min.
6. the preparation method of a kind of high surface microcapsules calcium hydroxide according to claim 1, it is characterized in that, in described step (5), described reaction condition is: with 4 ~ 6 DEG C/min temperature programming to 75 DEG C, stir 4 ~ 5h with 1000 ~ 1500r/min mixing speed, be cooled to room temperature.
7. the preparation method of a kind of high surface microcapsules calcium hydroxide according to claim 1, it is characterized in that, in described step (5), described drying condition is: vacuum 0.10 ~ 0.20MPa, temperature 70 ~ 90 DEG C, drying time 6 ~ 7h.
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| CN201510994804.2A CN105561899A (en) | 2015-12-28 | 2015-12-28 | Preparation method of high-surface-activity microcapsule calcium hydroxide |
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| CN201510994804.2A CN105561899A (en) | 2015-12-28 | 2015-12-28 | Preparation method of high-surface-activity microcapsule calcium hydroxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112341830A (en) * | 2020-11-09 | 2021-02-09 | 武汉理工大学 | Preparation method of self-packaging calcium alginate asphalt self-healing capsule |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1319681A1 (en) * | 2001-12-12 | 2003-06-18 | Degussa AG | PH controlled polyamide powder |
| CN104291371A (en) * | 2014-10-30 | 2015-01-21 | 杨富巍 | Preparation method for nanometer calcium hydroxide |
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- 2015-12-28 CN CN201510994804.2A patent/CN105561899A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1319681A1 (en) * | 2001-12-12 | 2003-06-18 | Degussa AG | PH controlled polyamide powder |
| CN104291371A (en) * | 2014-10-30 | 2015-01-21 | 杨富巍 | Preparation method for nanometer calcium hydroxide |
Non-Patent Citations (1)
| Title |
|---|
| 刘欣萍: "碱性无机粉体材料的研究——氢氧化钙的表面改性及其在塑料中阻燃性能的初步研究", 《中国优秀硕士学位论文全文数据库（电子期刊） 工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112341830A (en) * | 2020-11-09 | 2021-02-09 | 武汉理工大学 | Preparation method of self-packaging calcium alginate asphalt self-healing capsule |
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Application publication date: 20160511 |