CN114804180A - Method and device for preparing basic calcium chloride - Google Patents
Method and device for preparing basic calcium chloride Download PDFInfo
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- CN114804180A CN114804180A CN202210287948.4A CN202210287948A CN114804180A CN 114804180 A CN114804180 A CN 114804180A CN 202210287948 A CN202210287948 A CN 202210287948A CN 114804180 A CN114804180 A CN 114804180A
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- calcium chloride
- calcium
- preparing
- barrel
- microwave
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- 239000001110 calcium chloride Substances 0.000 title claims abstract description 36
- 229910001628 calcium chloride Inorganic materials 0.000 title claims abstract description 36
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 15
- 229960002713 calcium chloride Drugs 0.000 claims abstract description 34
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 33
- 239000010959 steel Substances 0.000 claims abstract description 33
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 20
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 20
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 19
- 229940052299 calcium chloride dihydrate Drugs 0.000 claims abstract description 18
- 238000000227 grinding Methods 0.000 claims abstract description 18
- LLSDKQJKOVVTOJ-UHFFFAOYSA-L calcium chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Ca+2] LLSDKQJKOVVTOJ-UHFFFAOYSA-L 0.000 claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 230000010355 oscillation Effects 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000007599 discharging Methods 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 12
- QFYUAKPQIZIUPT-UHFFFAOYSA-N [Ca].ClO Chemical compound [Ca].ClO QFYUAKPQIZIUPT-UHFFFAOYSA-N 0.000 claims description 7
- 238000005096 rolling process Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 3
- GRWPEXLRROVDML-UHFFFAOYSA-N [Ca].ClOCl Chemical compound [Ca].ClOCl GRWPEXLRROVDML-UHFFFAOYSA-N 0.000 claims 2
- 238000003801 milling Methods 0.000 claims 1
- 230000003534 oscillatory effect Effects 0.000 claims 1
- 239000000376 reactant Substances 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 229960005069 calcium Drugs 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 239000010881 fly ash Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229940043430 calcium compound Drugs 0.000 description 2
- 150000001674 calcium compounds Chemical class 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000004056 waste incineration Methods 0.000 description 1
Images
Classifications
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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
- C01F11/20—Halides
- C01F11/24—Chlorides
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/126—Microwaves
-
- 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
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crushing And Grinding (AREA)
Abstract
The invention discloses a method and a device for preparing basic calcium chloride, which can be used in the field of chemical industry, and the preparation is rapid and efficient, and the preparation method comprises the following steps: mixing and grinding calcium hydroxide and calcium chloride dihydrate, oscillating under the microwave condition, and drying after oscillation is finished to obtain basic calcium chloride; the preparation device comprises: the device comprises a grinding device, a microwave generator, an inclined steel cylinder, a quartz glass cylinder, a feeding hole and a discharging hole. The driving device in the middle of the cylinder rotates to drive the cylinder to rotate, raw materials are fed from the high end of the cylinder, and basic calcium chloride is discharged from the low end of the cylinder. The whole device can fully mix the reactants, improve the active components of the reactants and finally achieve the aim of quickly and efficiently preparing the basic calcium chloride.
Description
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to a method and a device for preparing basic calcium chloride.
Background
The waste incineration fly ash contains calcium hydroxide and chloride-containing calcium compounds, and many researches find that the incineration fly ash only contains one kind of basic calcium chloride containing the chloride-containing calcium compounds in the presence of the calcium hydroxide. The content of basic calcium chloride is very high, however, the current sale of alkali-free calcium chloride reagents causes inconvenience for the scientific research of fly ash and other basic calcium chloride. In addition, the basic calcium chloride can also be used as a calcium source to be added into animal feed. Therefore, the method for simply and quickly preparing the basic calcium chloride has scientific research value, industrial value and market prospect.
The Chinese patent 109198192A describes a new method for preparing basic calcium chloride, which is to dissolve a calcium source with hydrochloric acid, add an alkaline calcium source, stir at a constant temperature in a rake dryer for reaction, and dry after the reaction is finished, so as to obtain the basic calcium chloride. The preparation method of the basic calcium chloride introduced in the patent requires long reaction time and low reaction rate, reactants cannot be uniformly heated, and meanwhile, the basic calcium chloride is prepared by a wet method, the product needs to be dried, the energy consumption is high, and finally, the efficiency of preparing the basic calcium chloride is low.
Disclosure of Invention
In order to overcome the technical defects, the invention provides a method for preparing basic calcium chloride, which solves the problems related to the background art.
Accordingly, another technical problem to be solved by the present invention is to provide an apparatus for preparing basic calcium chloride.
As for the preparation method of basic calcium chloride, the preparation method of the present invention for solving the above technical problems comprises the following steps: mixing and grinding calcium hydroxide and calcium chloride dihydrate, oscillating under the microwave condition, and drying after oscillation is finished to obtain the basic calcium chloride. Preferably, the molar ratio of the calcium hydroxide to the calcium chloride dihydrate is (0.9-1.1): 1.
Preferably, the particle size of the calcium hydroxide and calcium chloride dihydrate is 0-500 μm.
Preferably, the grinding time of the method for preparing the basic calcium chloride is 6-9 minutes.
Preferably, the microwave power of the method for preparing the basic calcium chloride is 600-1000W, and the oscillation time is 3-5 minutes. Compared with the prior art, the invention has the beneficial effects that:
the contact area of reactants can be increased by mixing and grinding the calcium hydroxide and the calcium chloride dihydrate, so that a reaction system is activated and the reaction is promoted. The oscillation can make the reactant fully mixed, is favorable to improving the reaction rate. Meanwhile, the microwave frequency is high, the penetrating power is strong, on one hand, the calcium hydroxide and the calcium chloride dihydrate can be simultaneously heated inside and outside to achieve the purpose of rapid and uniform heating, on the other hand, the active components of the reactants can be promoted to be uniformly distributed on the carrier, so that the active components are highly dispersed on the surface of the carrier, and the microwave carrier has the advantages of short treatment time and the like.
As for the preparation device of the basic calcium chloride, the preparation device for solving the technical problem comprises a grinding device, a cylinder, a feeding machine, a calcium hydroxide feeding hole, a calcium chloride dihydrate feeding hole and a discharging hole; the cylinder body comprises a quartz glass cylinder body and two long cylinder bodies which are inclined inside and outside the steel cylinder body, a discharge hole and a low-end riding wheel supporting device are arranged at the low-end position of the cylinder body, a steel pipe elbow and a high-end riding wheel supporting device are arranged at the high-end position of the cylinder body, and a cylinder body driving device is also arranged in the middle of the cylinder body; a microwave generator is arranged on the outer side of the quartz glass cylinder; the calcium hydroxide feeding port and the calcium chloride dihydrate feeding port are connected with the feeding machine through the grinding device, and then the grinding device is connected with the steel pipe elbow through the feeding machine; the steel pipe elbow is connected with the steel cylinder through a rolling bearing; the discharge port is connected with the steel cylinder through a rolling bearing; the steel cylinder body is connected with the quartz glass cylinder body through a microwave generator; the steel cylinder body is connected with the riding wheel through a wheel belt.
By adopting the equipment with the structure, the quartz glass cylinder is adopted, and the microwave generator is arranged on the outer side of the cylinder, so that the calcium hydroxide and the calcium chloride dihydrate can be exposed to a microwave environment, and the aims of rapidly and uniformly heating and promoting the active components of reactants are fulfilled. And because the barrel is provided with the riding wheel and the barrel driving device, the barrel can perform rotary oscillation, so that reactants are fully mixed, and the reaction rate is improved.
The two long cylinders incline for 1-2 degrees along the horizontal direction.
The cylinder driving device comprises a driving motor, a gear and an outer gear ring.
The outer gear ring is fixedly arranged on the steel cylinder body.
The grinding device is a nano grinder, and the sample size of the nano grinder is 0-500 mu m.
The microwave generators are provided with a plurality of groups and are uniformly distributed on the outer side of the quartz glass cylinder.
Compared with the prior art, the invention has the beneficial effects that: the middle driving device arranged on the barrel rotates to drive the barrel to rotate, reactants are fed from the high end of the barrel, products are discharged from the low end of the barrel, the barrel is arranged to be inclined, and the reactants can perform sufficient chemical and physical reactions in the barrel at a certain speed.
Drawings
Fig. 1 is a schematic view of an apparatus for preparing basic calcium chloride in example 1.
Figure 2 XRD pattern of calcium chlorohydrate prepared in example 1. Wherein: 1-calcium hydroxide feed inlet; a feed inlet for 2-calcium chloride dihydrate; 3-a grinding device; 4-a feeder; 5-a belt wheel; 6-external gear ring; 7-a microwave generator; 8-a discharge hole; 9-steel pipe elbow; 10-a second riding wheel supporting device; 11-a drive motor; 12-a gear; 13-a steel cylinder; 14-quartz glass cylinder; 15-a first riding wheel supporting device; 16-a first rolling bearing; 17-a second rolling bearing.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The invention provides a method for preparing basic calcium chloride, which comprises the following steps:
10kg of calcium hydroxide and 19.865kg of calcium chloride dihydrate (commercially available raw materials) were fed into the mill from the feed inlet in a molar ratio of 1:1, respectively, and the mill was started for 8 minutes. After the grinding is finished, the feeder is opened, the reaction raw materials enter the quartz glass cylinder through the steel pipe elbow, the microwave generator and the cylinder driving device are started, the microwave power is adjusted to be 600W, and the oscillation time is 4 minutes. And opening a discharge port valve after oscillation is finished, sending the product into a vacuum drying oven, and drying for 1h at the temperature of 100 ℃ to finally obtain the high-purity basic calcium chloride particles.
The invention provides a device for preparing basic calcium chloride, which is shown in figure 1: comprises a grinding device (3), an inclined steel cylinder (13), a quartz glass cylinder (14), a feeder (4), a calcium hydroxide feed port (1), a calcium chloride dihydrate feed port (2) and a discharge port (8); the grinding device (3) is a nano grinder; the inclination of the steel cylinder (13) and the quartz glass cylinder (14) is 1-2 degrees; the steel cylinder body (13) is connected with the steel pipe elbow (9) and the discharge hole (8) through a rolling bearing, and the steel cylinder body (13) is connected with the riding wheel through a wheel belt (5).
The steel cylinder is characterized in that a discharge hole (8) and a low-end supporting roller supporting device (15) are arranged at the low end of the steel cylinder, a steel pipe elbow (9) and a high-end supporting roller supporting device (10) are arranged at the high end of the steel cylinder, and a cylinder driving device is further arranged in the middle of the cylinder.
The cylinder driving device comprises a driving motor (11), a gear (12) and an outer gear ring (6); the outer gear ring (6) is fixedly arranged on the steel cylinder body (13).
Comprises a microwave generator (7); the multiple groups of microwave generators (7) are uniformly distributed on the outer side of the quartz glass cylinder body (14); the steel cylinder (13) is connected with the quartz glass cylinder (14) through a microwave generator (7).
The purity of the target product basic calcium chloride obtained in the embodiment is 99.1% by detection, and the product spectrum in the XRD spectrum of the product is consistent with the standard spectrum by XRD detection.
Claims (13)
1. A method for preparing basic calcium chloride is characterized by comprising the following steps: mixing and grinding calcium hydroxide and calcium chloride dihydrate, oscillating under the microwave condition, and drying after oscillation is finished to obtain the basic calcium chloride.
2. A process for preparing calcium chlorohydrate according to claim 1, wherein the particle size of the calcium hydroxide and calcium chloride dihydrate is in the range of 0 to 500 μm.
3. A process for preparing calcium chlorohydrate according to claim 1, wherein the calcium hydroxide is mixed with the calcium chloride dihydrate in a molar ratio of (0.9-1.1): 1.
4. A process for preparing calcium chlorohydrate according to claim 1, wherein the milling time is from 6 to 9 minutes.
5. The method for preparing basic calcium chloride according to claim 1, wherein the microwave power is 600-1000W, and the oscillation time is 3-5 minutes.
6. The method according to any one of claims 1 to 5, wherein the oscillatory reaction is carried out in a microwave rotary device, and the specific process comprises the following steps: respectively adding calcium hydroxide and calcium chloride dihydrate from a feed inlet of a microwave rotary device, starting a microwave generator to a specified power, starting a driving device to perform microwave oscillation reaction, and directly discharging at a discharge port of the microwave rotary device after the reaction is finished to obtain the basic calcium chloride.
7. A device for preparing basic calcium chloride comprises a grinding device (3), a barrel, a feeder (4), a microwave generator (7), a calcium hydroxide feed inlet (1), a calcium chloride dihydrate feed inlet (2) and a discharge outlet (8), and is characterized in that the barrel comprises a quartz glass barrel (14) and a steel barrel (13), wherein the two long barrels are inclined inside and outside the barrel, the lower end of the barrel is provided with the discharge outlet (8) and a lower end riding wheel supporting device (15), the higher end of the barrel is provided with a steel pipe elbow (9) and a higher end riding wheel supporting device (10), the middle of the barrel is also provided with a barrel driving device, the microwave generator (7) is arranged outside the quartz glass barrel, the calcium hydroxide feed inlet and the calcium chloride dihydrate feed inlet are connected with the feeder (4) through the grinding device (3), and then the grinding device is connected with the steel pipe elbow (9) through the feeder (4), the steel pipe elbow (9) is connected with the steel cylinder body (13) through a rolling bearing (16), the discharge port (8) is connected with the steel cylinder body (13) through the rolling bearing (16), the steel cylinder body (13) is connected with the quartz glass cylinder body (14) through a microwave generator (7), and the steel cylinder body (13) is connected with the riding wheel through a wheel belt (5).
8. The apparatus for preparing calcium chlorohydrate of claim 7, wherein the two elongated barrels are inclined at 1-2 degrees in the horizontal direction.
9. Device for preparing calcium oxychloride as claimed in claim 7, wherein the cartridge drive comprises a drive motor (11), a gear (12) and an external gear ring (6).
10. Device for the preparation of calcium oxychloride as claimed in claim 7, wherein the outer ring gear (6) is fixedly mounted on the steel cylinder (13).
11. An apparatus for preparing calcium chlorohydrate according to claim 7, wherein the microwave generators (7) are provided in a plurality of groups, and are uniformly distributed outside the quartz glass cylinder (14).
12. An apparatus for preparing calcium chlorohydrate according to claim 7, wherein the grinding apparatus (3) is a nano-mill.
13. The nano-mill according to claim 11, wherein the nano-mill has a grain size of 0 to 500 μm.
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CN202210287948.4A CN114804180A (en) | 2022-03-23 | 2022-03-23 | Method and device for preparing basic calcium chloride |
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2441337A (en) * | 1942-12-30 | 1948-05-11 | Pennsylvania Salt Mfg Co | Process of preparing dibasic calcium hypochlorite |
CN101941719A (en) * | 2010-05-25 | 2011-01-12 | 河北科技大学 | Method for combined production of ammonia and basic calcium chloride by decomposing ammonium chloride |
CN109198191A (en) * | 2018-10-30 | 2019-01-15 | 长沙兴嘉生物工程股份有限公司 | A kind of preparation method and applications of hydroxy chloride calcium |
CN109198192A (en) * | 2018-10-30 | 2019-01-15 | 长沙兴嘉生物工程股份有限公司 | The preparation method and applications of hydroxy chloride calcium |
CN217627645U (en) * | 2022-03-23 | 2022-10-21 | 南京师范大学镇江创新发展研究院 | Microwave rotating device for preparing basic calcium chloride |
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2022
- 2022-03-23 CN CN202210287948.4A patent/CN114804180A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2441337A (en) * | 1942-12-30 | 1948-05-11 | Pennsylvania Salt Mfg Co | Process of preparing dibasic calcium hypochlorite |
CN101941719A (en) * | 2010-05-25 | 2011-01-12 | 河北科技大学 | Method for combined production of ammonia and basic calcium chloride by decomposing ammonium chloride |
CN109198191A (en) * | 2018-10-30 | 2019-01-15 | 长沙兴嘉生物工程股份有限公司 | A kind of preparation method and applications of hydroxy chloride calcium |
CN109198192A (en) * | 2018-10-30 | 2019-01-15 | 长沙兴嘉生物工程股份有限公司 | The preparation method and applications of hydroxy chloride calcium |
CN217627645U (en) * | 2022-03-23 | 2022-10-21 | 南京师范大学镇江创新发展研究院 | Microwave rotating device for preparing basic calcium chloride |
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