CN102992292A - Production technology and application of calcium hydrophosphate - Google Patents
Production technology and application of calcium hydrophosphate Download PDFInfo
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- CN102992292A CN102992292A CN2012105622543A CN201210562254A CN102992292A CN 102992292 A CN102992292 A CN 102992292A CN 2012105622543 A CN2012105622543 A CN 2012105622543A CN 201210562254 A CN201210562254 A CN 201210562254A CN 102992292 A CN102992292 A CN 102992292A
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Abstract
The invention relates to a production technology and application of calcium hydrophosphate. The production technology comprises the following steps of: by using an ammonium dibasic phosphate and a calcium chloride solution as raw materials, carrying out double liquid phases to obtain hydryoxyapetite by stirring at a certain temperature and flow rate, then dewatering through a belt filter to separate and washing a mother liquid till chloride ions reach 500PPM, thus obtaining hydryoxyapetite; adding a certain amount of deionized water to hydryoxyapetite, adjusting a slurry ratio to be in line with technological requirements, adding a certain amount of acid, carrying out high-temperature digestion after adjusting a pH value, observing the state of the slurry after raising the temperature to 90 DEG C, stopping heating when the slurry is expanded and solidified, and removing two crystal water after settling for 30 minutes, thereby obtaining calcium phosphate dibasic anhydrous; carrying out washing chlorine, dewatering, drying and sieving, thus obtaining the calcium hydrophosphate finished product. The production technology has the advantages that the synthetic technology is simple, raw materials are easily obtained, by-products can be recycled, and the environmental pollution is little.
Description
Technical field
The invention belongs to the secondary calcium phosphate preparation field, relate to particularly a kind of production technique and application of secondary calcium phosphate.
Background technology
The mode of the existing secondary calcium phosphate (being calcium monohydrogenphosphate) of producing is various, although the content of its ratio of calcium and phosphorus and various impurity can reach the requirement of producing halogen calcium phosphate fluoressent powder, but because secondary calcium phosphate accounts for the ratio more than 80% in the preparation of halogen calcium phosphate fluoressent powder, it is the skeleton of fluorescent material, so the crystal formation to secondary calcium phosphate requires harsh, imperfect and thin flat secondary calcium phosphate crystal formation, can affect light-emitting phosphor brightness, increase light decay, reduce quality and the work-ing life of fluorescent material, and the synthetic secondary calcium phosphate of existing secondary calcium phosphate synthesis mode, the shape of its particle can't satisfy this requirement.
Summary of the invention
Produce secondary calcium phosphate without the problem of crystal formation in order to have solved other modes, the purpose of this invention is to provide a kind of production technique and application of secondary calcium phosphate, this technique synthesis technique is simple, and raw material is easy to get, the by product recoverable, and environmental pollution is little.
The invention provides a kind of production technique of secondary calcium phosphate, this technological process is:
(1) be starting material with ammonium dibasic phosphate solution and calcium chloride solution, be under the 1:1.05 condition stirs in 28-35 ℃ of temperature and volumetric flow rate, Two Liquid Phases synthesizes dicalcium phosphate dihydrate, after through band filter dehydration mother liquor separate, washing reaches 500PPM to chlorion, namely obtains dicalcium phosphate dihydrate;
(2) add deionized water in dicalcium phosphate dihydrate, being modulated into slurry proportion is 1.0-1.2, and adds a certain amount of acid, regulate the pH value behind 4-5, carry out the high temperature digestion, after temperature is raised to 90 ℃, observe slurry form, when find slurry swollen solid after, stopped heating, carry out sedimentation after 30 minutes, take off two crystal water, obtain calcium phosphate dibasic anhydrous, wash again chlorine, dehydration, oven dry after sieving, obtains the secondary calcium phosphate finished product.
The production technique of secondary calcium phosphate provided by the invention, in the step (1), described ammonium dibasic phosphate solution concentration is 2.5mol/L, the pH value is 7-8.Described calcium chloride solution concentration is 2.5mol/L, and the pH value is 4-6.
The production technique of secondary calcium phosphate provided by the invention, the granularity of described calcium phosphate dibasic anhydrous are D50:9-10.5 μ, below the D99:25 μ.
The production technique of secondary calcium phosphate provided by the invention, the crystal formation of described calcium phosphate dibasic anhydrous are square tabular.
The secondary calcium phosphate that technique provided by the invention is prepared is applied to prepare fluorescent material.
Key point of the present invention is the two step synthesis secondary calcium phosphate.The first step is building-up process, priority control synthesis temperature, pH value and washing.Second step is high temperature dehydration, priority control slurry ratio, pH value and heat-up rate and swollen solid state.
The secondary calcium phosphate that two step synthesis technology mode of the present invention makes has unique square platy structure, can observe at microscopically, and the complete in crystal formation of hydrogen calcium, neat, evenly, have certain thickness, be to be exclusively used in the halogen calcium phosphate fluoressent powder preparation to use.The fluorescent material that the secondary calcium phosphate sintering that uses the present invention to make goes out has complete crystalline structure, and optical throughput is high, and light decay is little.Synthesis technique of the present invention is simple, and raw material is easy to get, the by product recoverable, and environmental pollution is little.
Embodiment
The following examples will be further described the present invention, but not thereby limiting the invention.
Embodiment 1
One, the preparation of solution:
Ammonium dibasic phosphate solution: concentration: 2.5mol/L
PH value: 7.6
Temperature: 30 ℃
Calcium chloride solution: concentration: 2.5mol/L
PH value: 5.0
Temperature: 30 ℃
Two, synthesize, wash, size mixing
1, in first synthesis tank (two synthesis tanks are continuous), fills with deionized water first, open stirring.Open according to demand the under meter of ammonium dibasic phosphate solution and calcium chloride solution, flow is respectively 800L/ hour, 840L/ hour, 30 ℃ of synthesis temperatures.
2, when second synthesis tank filled with slurry, open band filter and carry out the mother liquor separation, start simultaneously washing device material cake (dicalcium phosphate dihydrate) is washed, make material cake chloride ion-containing below 500PPM.The material cake falls into the recycled pulp batch can from filter cloth.
3, adjust the injected water flow, the slurry proportion that makes recycled pulp is 1.0-1.2.
Three, the washing of the dehydration of dicalcium phosphate dihydrate, secondary calcium phosphate, oven dry screening.
1, the slurry of dicalcium phosphate dihydrate is squeezed in the retort, opened stirring, add hydrochloric acid or phosphoric acid adjust pH to 4.5.Open steam valve, heat, after temperature is raised to 90 ℃, observe slurry form, when find slurry swollen solid after, stopped heating carried out sedimentation after 30 minutes, took off two crystal water, obtained calcium phosphate dibasic anhydrous.
2, calcium phosphate dibasic anhydrous is washed, dewatered drying, the screening both the secondary calcium phosphate finished product.
Four, assay
1, crystal formation: square tabular.
2, granularity: D50:9.5 μ, D10; 4.2 μ, D99; 24.7 μ.
Claims (6)
1. the production technique of a secondary calcium phosphate, it is characterized in that: this technological process is:
(1) be starting material with ammonium dibasic phosphate solution and calcium chloride solution, be under 1: 1.05 condition stirs in 28-35 ℃ of temperature and volumetric flow rate, Two Liquid Phases synthesizes dicalcium phosphate dihydrate, after through band filter dehydration mother liquor separate, washing reaches 500PPM to chlorion, namely obtains dicalcium phosphate dihydrate;
(2) add deionized water in dicalcium phosphate dihydrate, being modulated into slurry proportion is 1.0-1.2, and adds a certain amount of acid, regulate the pH value behind 4-5, carry out the high temperature digestion, after temperature is raised to 90 ℃, observe slurry form, when find slurry swollen solid after, stopped heating, carry out sedimentation after 30 minutes, take off two crystal water, obtain calcium phosphate dibasic anhydrous, wash again chlorine, dehydration, oven dry after sieving, obtains the secondary calcium phosphate finished product.
2. according to the production technique of the described secondary calcium phosphate of claim 1, it is characterized in that: in the step (1), described ammonium dibasic phosphate solution concentration is 2.5mol/L, and the pH value is 7-8.
3. according to the production technique of the described secondary calcium phosphate of claim 1, it is characterized in that: in the step (1), described calcium chloride solution concentration is 2.5mol/L, and the pH value is 4-6.
4. according to the production technique of the described secondary calcium phosphate of claim 1, it is characterized in that: in the step (2), the granularity of described calcium phosphate dibasic anhydrous is D50:9-10.5 μ, below the D99:25 μ.
5. according to the production technique of the described secondary calcium phosphate of claim 1, it is characterized in that: in the step (2), the crystal formation of described calcium phosphate dibasic anhydrous is square tabular.
6. the secondary calcium phosphate prepared of the described technique of claim 1 is applied to prepare fluorescent material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105622543A CN102992292A (en) | 2012-12-21 | 2012-12-21 | Production technology and application of calcium hydrophosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105622543A CN102992292A (en) | 2012-12-21 | 2012-12-21 | Production technology and application of calcium hydrophosphate |
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| Publication Number | Publication Date |
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| CN102992292A true CN102992292A (en) | 2013-03-27 |
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| CN2012105622543A Pending CN102992292A (en) | 2012-12-21 | 2012-12-21 | Production technology and application of calcium hydrophosphate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103738933A (en) * | 2013-12-13 | 2014-04-23 | 江苏晓春新材料有限公司 | Method for recovering high purity calcium hydrogen phosphate in sulfur acid-containing waste phosphoric acid |
| CN106395781A (en) * | 2016-08-31 | 2017-02-15 | 金华 | Novel dehydration method of calcium hydrogen phosphate product slurry |
-
2012
- 2012-12-21 CN CN2012105622543A patent/CN102992292A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 小沢利之等: "磷酸氢钙二水合物在水中的脱水作用", 《日用化学工业译丛》 * |
| 缪兴邦: "透明片状磷酸氢钙晶体的制备", 《化学世界》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103738933A (en) * | 2013-12-13 | 2014-04-23 | 江苏晓春新材料有限公司 | Method for recovering high purity calcium hydrogen phosphate in sulfur acid-containing waste phosphoric acid |
| CN106395781A (en) * | 2016-08-31 | 2017-02-15 | 金华 | Novel dehydration method of calcium hydrogen phosphate product slurry |
| CN106395781B (en) * | 2016-08-31 | 2018-11-09 | 金华 | The dewatering of calcium monophosphate product slurry |
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Application publication date: 20130327 |