CN106512661A - Method and device for circulating ammonia gas in hydroxyapatite preparation process - Google Patents
Method and device for circulating ammonia gas in hydroxyapatite preparation process Download PDFInfo
- Publication number
- CN106512661A CN106512661A CN201610963447.8A CN201610963447A CN106512661A CN 106512661 A CN106512661 A CN 106512661A CN 201610963447 A CN201610963447 A CN 201610963447A CN 106512661 A CN106512661 A CN 106512661A
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- ammonia
- hydroxyapatite
- tourie
- reactor
- phosphoric acid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/10—Inorganic absorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/40—Nitrogen compounds
- B01D2257/406—Ammonia
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method and a device for circulating ammonia gas in the hydroxyapatite preparation process, and aims to produce hydroxyapatite by circulating ammonium phosphate which is produced through reaction of the ammonia gas and diluted phosphoric acid. The device comprises a size mixing tank, a reaction kettle, a condenser, a gas-liquid separator, an ammonia gas absorption tank, a magnetic pump and a vacuum pump, wherein the reaction kettle and the ammonia gas absorption tank form a circulation loop through connecting tubes and the magnetic pump; the ammonia gas absorption tank is filled with diluted phosphoric acid; a micro pore aeration disc is arranged on a coiled tube at the bottom of the ammonia absorption tank; the ammonia gas forms bubbles being about 2mm after passing through the micro pore aeration disc and sufficiently contacts and reacts with the diluted phosphoric acid; an ammonium phosphate solution obtained through the reaction is pumped back into the reaction kettle through the magnetic pump to be circulated and reacted. By adopting the method and the device, cleaner production can be achieved, the consequence that the environment is polluted or the treatment cost is increased because of improper ammonia gas treatment can be avoided, the micro pore aeration disc is small and dense in aperture and high in absorption efficiency, the whole device is simple in structure and convenient to operate, environment pollution cannot be caused by waste gases, the production cost of hydroxyapatite can be lowered, and the device is worthy of popularization.
Description
Technical field
The present invention relates to one kind prepares exhaust gas treatment technology during hydroxyapatite, hydroxyapatite mistake is especially prepared
Method and its device that in journey, ammonia recycle is utilized.
Background technology
Hydroxyapatite is chemically combined to form by calcium and phosphate.The method for preparing hydroxyapatite is a lot,
But every kind of method is all that wherein ammonium phosphate salt is due to containing being equipped with synthesis material according to the calcium phosphorus atoms ratio of hydroxyapatite 1.67
There is generation of the ammonia radical ion to hydroxyapatite to have facilitation, become optimal phosphorus source and select.The participation of ammonium phosphate salt is anti-
The generation of by-product ammonia should be necessarily had, substantial amounts of ammonia brings certain impact to operating environment, and cost recovery is high.Mesh
It is front mostly as waste gas discharge or by emission treatment after water absorption, not only waste of resource can also cause certain dirt to environment
Dye.Rationally how the difficult problem that faces in a production process using the ammonia in hydroxyapatite production.
The content of the invention
Process for the existing by-product ammonia for preparing hydroxyapatite generation arbitrarily discharge or water absorption and there is ring
The defect such as border pollution or cost height, the invention provides preparation method and its dress that ammonia recycle during hydroxyapatite is utilized
Put, its technical scheme is as follows：
The method that ammonia is recycled during preparing hydroxyapatite, it is characterised in that comprise the following steps：
(1) in reactor raw material calcium, ammonium phosphate salt, stirring reaction is added to prepare hydroxyl phosphorus with calcium phosphorus atoms ratio as 1.67
Lime stone；
(2) collect ammonia and the vapor produced during hydroxyapatite is prepared；
(3) ammonia in separation above-mentioned steps (2), vapor；
(4) water vapor condensation Cheng Shui isolated in above-mentioned steps (3) is back in reactor keeps reactant dense
That what is spent is constant；
(5) using vacuum pump by ammonia pump isolated in step (3) to ammonia tourie, in the ammonia tourie
Equipped with phosphoric acid,diluted；
(6), after the phosphoric acid,diluted and ammonia in by ammonia tourie reacts completely, obtain ammonium phosphate salt solution；
(7) will be circulated the ammonium phosphate salt solution obtained in above-mentioned steps (6) using magnetic drive pump in its blowback reactor is made
With.
In order to realize the above-mentioned method that ammonia is recycled during hydroxyapatite is prepared, skill of the present invention
Art scheme is as follows：
A kind of device suitable for ammonia is recycled during hydroxyapatite is prepared, it is characterised in that：Including tune
Slurry tank, reactor, condenser, gas-liquid separator, ammonia tourie, magnetic drive pump, vacuum pump, the reactor top is provided with charging
Mouth, gas outlet, the charging aperture are connected with tank of sizing mixing by connecting tube, the sizing mixing magnetic drive pump of be provided between tank and reactor, institute
State, the gas outlet connects the air inlet on condenser top, the condenser bottom by connecting tube
End is provided with separating opening, and the separating opening is connected with gas-liquid separator by connecting tube, and the gas-liquid separator bottom is provided with condensation
Water separating opening, the condensed water separating opening are connected to be formed with the connecting tube of the gas outlet on reactor top by connecting tube and loop back
Road, the gas-liquid separator top are provided with ammonia separating opening, and the ammonia separating opening absorbs upper end with ammonia by connecting tube
The connection of ammonia air inlet, the ammonia air inlet is connected with breather, and the breather is located at ammonia tourie bottom, the ammonia
The breather of gas bottom is coil arrangement, and the coil pipe is provided with microporous aeration disc, and the ammonia tourie bottom is provided with out liquid
Mouthful, the liquid outlet is connected to form ammonia recycle loop by connecting tube and reactor top, and the reactor and ammonia absorb
Magnetic drive pump is provided between tank.
Further, in order to improve the absorbance of ammonia, the ammonia tourie is two of one or series connection.
Further, in order that ammonia is fully contacted with phosphoric acid,diluted, fully absorb, the microporous aeration disc that the ammonia passes through
Aperture is 2mm.
Further, in order to recycle ammonia, the ammonia tourie is equipped with phosphoric acid,diluted, ammonia and phosphoric acid,diluted reaction life
Use into ammonium phosphate salt as feedstock circulation.
Further, in order that ammonia and phosphoric acid,diluted are fully contacted, in the ammonia tourie, the liquid level of phosphoric acid,diluted is higher than
Microporous aeration disc.
Further, in order to ammonia is caused ammonia tourie, the ammonia absorbs upper end and is connected with vacuum pump.
The device have the advantages that as follows：
Invention proposition prepares the circulation utilization method and its device of hydroxyapatite byproduct in process thing ammonia, by by ammonia
Gas and phosphoric acid,diluted reaction generate ammonium phosphate salt, are circulated production as the raw material for preparing hydroxyapatite.The method is by setting
Ammonia tourie is put, and it is breather coil pipe to be arranged in ammonia tourie bottom, by setting up microporous aeration disc on coil pipe pipe shaft
Come the phosphoric acid,diluted haptoreaction in realizing ammonia gas and tourie.The aperture of microporous aeration disc is small and dense, and ammonia passes through micropore
Aeration plate forms the bubble of 2mm, is fully contacted reaction with the phosphoric acid,diluted in tourie.Directly open on pipe shaft relative to existing
Hole technology, not only processing difficulties, high processing costs, and open pore size are also very big, ammonia by when can be because volume be crossed very much not
Beneficial to fully reacting with phosphoric acid,diluted.Meanwhile, apparatus of the present invention utilize condenser and gas-liquid separator, efficiently separated vapor and
Ammonia, condensed water are back to reactor, not only realize and separate with ammonia, and maintain the reactant in reactor
Constant concentration.The ammonia being separated from water, can enter ammonia tourie in the presence of vacuum pump, be inhaled by the phosphoric acid,diluted in tourie
Harvest ammonium phosphate salt, becomes raw material with use to be recycled.Whole device simple structure, easy to operate, waste gas does not result in environment
Pollution, while will not also improve cost recovery, realizes clean manufacturing, reduces the production cost of hydroxyapatite, be worth pushing away
Extensively.
Description of the drawings
Fig. 1 prepares hydroxyapatite and recycles ammonia apparatus structure schematic diagram.
Two ammonia tourie cascaded structure schematic diagrams of Fig. 2.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.It is based on
Embodiment in the present invention, those of ordinary skill in the art obtained on the premise of creative work is not made it is all its
His embodiment, belongs to protection scope of the present invention.
In order to reach the purpose of the present invention, as Figure 1-Figure 2, ammonia is recycled during preparing hydroxyapatite
Method, it is characterised in that comprise the following steps：
(1) in reactor raw material calcium, ammonium phosphate salt, stirring reaction is added to prepare hydroxyl phosphorus with calcium phosphorus atoms ratio as 1.67
Lime stone；
(2) collect ammonia and the vapor produced during hydroxyapatite is prepared；
(3) ammonia in separation above-mentioned steps (2), vapor；
(4) water vapor condensation Cheng Shui isolated in above-mentioned steps (3) is back in reactor keeps reactant dense
That what is spent is constant；
(5) using vacuum pump by ammonia pump isolated in step (3) to ammonia tourie, in the ammonia tourie
Equipped with phosphoric acid,diluted；
(6) after phosphoric acid,diluted and ammonia in ammonia tourie react completely, obtain ammonium phosphate salt solution；
(7) will be circulated the ammonium phosphate salt solution obtained in above-mentioned steps (6) using magnetic drive pump in its blowback reactor is made
With.
In order to realize the above-mentioned method that ammonia is recycled during hydroxyapatite is prepared, skill of the present invention
Art scheme is as follows：A kind of device suitable for ammonia is recycled during hydroxyapatite is prepared, it is characterised in that：Including
Size mixing tank 1, reactor 2, condenser 3, gas-liquid separator 4, ammonia tourie 5, magnetic drive pump 6, vacuum pump 7, the reactor 2 is pushed up
End is provided with charging aperture, gas outlet, and the charging aperture is connected with tank 1 of sizing mixing by connecting tube 8, described to size mixing between tank 1 and reactor 2
Magnetic drive pump 6 is provided with, agitator 9 in the reactor 2, is provided with, the gas outlet connects entering for 3 top of condenser by connecting tube 8
QI KOU, 3 bottom of the condenser are provided with separating opening, and the separating opening is connected with gas-liquid separator 4 by connecting tube 8, the gas
4 bottom of liquid/gas separator is provided with condensed water separating opening, and the condensed water separating opening is by connecting tube 8 and the outlet on 2 top of reactor
The connection of connecting tube 8 of mouth forms closed circuit, and 4 top of the gas-liquid separator is provided with ammonia separating opening, the ammonia separating opening
It is connected with the ammonia air inlet on 5 top of ammonia tourie by connecting tube 8, the ammonia air inlet is connected with breather 10, described
Breather 10 is located at 5 bottom of ammonia tourie, and the breather 10 of 5 bottom of ammonia tourie is coil arrangement, the coil pipe
Microporous aeration disc 11 is provided with, 5 bottom of ammonia tourie is provided with liquid outlet, and the liquid outlet is by connecting tube 8 and reaction
2 top of kettle is connected to form ammonia recycle loop, and magnetic drive pump 6 is provided between the reactor 2 and ammonia tourie 5.
Preferably, the ammonia tourie 5 is two of one or series connection.
Preferably, 11 aperture of the microporous aeration disc is 2mm.
Preferably, the ammonia tourie 5 is equipped with phosphoric acid,diluted.
Preferably, in the ammonia tourie 5, the liquid level of phosphoric acid,diluted is higher than microporous aeration disc.
Preferably, 5 top of ammonia tourie is connected with vacuum pump 7.
Its specific embodiment is：As shown in figure 1, when preparing hydroxyapatite, first adding raw materials into tank 1 of sizing mixing, raw material
After being sufficiently mixed uniformly, the raw material sized mixing in tank 1 is pumped in reactor 2 using magnetic drive pump 6.Start the stirring in reactor 2
Device 9, is stirred reaction.During the course of the reaction, by-product ammonia, is entered by the gas outlet on 2 top of reactor with vapor
Enter condenser 3, vapor is changed into liquid to the cold, and ammonia is entered in gas-liquid separator 4 together.The gravity of utilization of condensed water itself
4 bottom of gas-liquid separator is fallen into, is entered by condensed water separating opening, connecting tube 8 and in reactor 2, is kept the concentration of reactant steady
It is fixed.Meanwhile, ammonia enters ammonia tourie 5 by the ammonia separating opening on 4 top of gas-liquid separator.Now, in ammonia tourie
Dilute phosphoric acid solution be higher than tank bottoms microporous aeration disc 11, close the valve of ammonia tourie bottom, it is ensured that ammonia tourie
Sealing.Start vacuum pump 7, by ammonia suction tank, ammonia forms 2mm through breather 10, coil pipe, microporous aeration disc 11
The minute bubbles of left and right, the phosphoric acid,diluted contact fully and in tank body are further absorbed, and form ammonium phosphate salt.After absorption is finished, open
Ammonia absorbs the valve of pot bottom, using magnetic drive pump 6 by ammonium phosphate salt solution blowback reactor 2, participates in hydroxyapatite
Prepare, so as to realize recycling for by-product ammonia.In order to further improve the absorption efficiency of ammonia, and avoid first
Ammonia coefficient pipe ammonia after saturation is absorbed leaks, and the ammonia tourie that can connect same behind ammonia tourie is used as peace
Full tank is used, as shown in Fig. 2 the ammonia absorbance of two section ammonia touries is up to more than 95%.
The above, the only specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, any
Those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, should all be contained
Cover within protection scope of the present invention.Therefore, protection scope of the present invention should be defined by the scope of the claims.
Claims (7)
1. the method that ammonia is recycled during preparing hydroxyapatite, it is characterised in that comprise the following steps：
(1) in reactor raw material calcium, ammonium phosphate salt, stirring reaction is added to prepare hydroxy-apatite with calcium phosphorus atoms ratio as 1.67
Stone；(2) collect ammonia and the vapor produced during hydroxyapatite is prepared；
(3) ammonia in separation above-mentioned steps (2), vapor；
(4) water vapor condensation Cheng Shui isolated in above-mentioned steps (3) is back in reactor and keeps reactant concentration
It is constant；(5) using vacuum pump by ammonia pump isolated in step (3) to ammonia tourie, fill in the ammonia tourie
There is phosphoric acid,diluted；
(6) after phosphoric acid,diluted and ammonia in ammonia tourie react completely, obtain ammonium phosphate salt solution；
(7) the ammonium phosphate salt solution obtained in above-mentioned steps (6) will be recycled in its blowback reactor using magnetic drive pump.
2. a kind of device suitable for ammonia is recycled during hydroxyapatite is prepared, it is characterised in that：Including sizing mixing
Tank, reactor, condenser, gas-liquid separator, ammonia tourie, magnetic drive pump, vacuum pump, the reactor top are provided with charging
Mouth, gas outlet, the charging aperture are connected with tank of sizing mixing by connecting tube, the sizing mixing magnetic drive pump of be provided between tank and reactor, institute
State, the gas outlet connects the air inlet on condenser top, the condenser bottom by connecting tube
End is provided with separating opening, and the separating opening is connected with gas-liquid separator by connecting tube, and the gas-liquid separator bottom is provided with condensation
Water separating opening, the condensed water separating opening are connected to be formed with the connecting tube of the gas outlet on reactor top by connecting tube and loop back
Road, the gas-liquid separator top are provided with ammonia separating opening, and the ammonia separating opening absorbs upper end with ammonia by connecting tube
The connection of ammonia air inlet, the ammonia air inlet is connected with breather, and the breather is located at ammonia tourie bottom, the ammonia
The breather of gas bottom is coil arrangement, and the coil pipe is provided with microporous aeration disc, and the ammonia tourie bottom is provided with out liquid
Mouthful, the liquid outlet is connected to form ammonia recycle loop by connecting tube and reactor top, and the reactor and ammonia absorb
Magnetic drive pump is provided between tank.
3. a kind of device suitable for ammonia is recycled during hydroxyapatite is prepared as claimed in claim 2, its
It is characterised by：The ammonia tourie is two of one or series connection.
4. a kind of device suitable for ammonia is recycled during hydroxyapatite is prepared as claimed in claim 2, its
It is characterised by：The microporous aeration disc aperture is 2mm.
5. a kind of device suitable for ammonia is recycled during hydroxyapatite is prepared as claimed in claim 2, its
It is characterised by：The ammonia tourie is equipped with phosphoric acid,diluted.
6. a kind of device suitable for ammonia is recycled during hydroxyapatite is prepared as claimed in claim 2, its
It is characterised by：In the ammonia tourie, the liquid level of phosphoric acid,diluted is higher than microporous aeration disc.
7. a kind of device suitable for ammonia is recycled during hydroxyapatite is prepared as claimed in claim 2, its
It is characterised by：The ammonia absorbs upper end and is connected with vacuum pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610963447.8A CN106512661A (en) | 2016-10-28 | 2016-10-28 | Method and device for circulating ammonia gas in hydroxyapatite preparation process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610963447.8A CN106512661A (en) | 2016-10-28 | 2016-10-28 | Method and device for circulating ammonia gas in hydroxyapatite preparation process |
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| Publication Number | Publication Date |
|---|---|
| CN106512661A true CN106512661A (en) | 2017-03-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610963447.8A Pending CN106512661A (en) | 2016-10-28 | 2016-10-28 | Method and device for circulating ammonia gas in hydroxyapatite preparation process |
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB730574A (en) * | 1951-05-18 | 1955-05-25 | Kestner App Evaporateurs | Improvements in or relating to the manufacture of diammonium phosphate in pulverulent form |
| CN101249313A (en) * | 2008-04-01 | 2008-08-27 | 南京特种气体厂有限公司 | Recovery cyclic utilization method and apparatus for recovering discharged alkaline air in process of production of silicone hydride with magnesium silicide method |
| CN101607719A (en) * | 2008-06-20 | 2009-12-23 | 南通江山农药化工股份有限公司 | The clean reclaiming process of ammonia gas as byproduct of glyphosate |
| CN101613338A (en) * | 2009-07-21 | 2009-12-30 | 西安交通大学 | A kind of preparation method of cyclic carbonate of while coproduction ammonium hydrogen phosphate |
| CN101773684A (en) * | 2010-03-19 | 2010-07-14 | 西南大学 | Preparation method of fibroin/hydroxyapatite porous scaffold |
| CN202054624U (en) * | 2011-04-28 | 2011-11-30 | 杭州胜大药业有限公司 | Ammonia gas recycling device for nicotinic acid process |
| CN102319534A (en) * | 2011-08-25 | 2012-01-18 | 江西金达莱环保研发中心有限公司 | Method for exhaust gas purification |
| CN202366608U (en) * | 2011-12-20 | 2012-08-08 | 厦门市格绿科技有限公司 | Ammonia recovery device |
| CN203577568U (en) * | 2013-11-27 | 2014-05-07 | 上海众一石化工程有限公司 | Tail gas recycling device |
| CN206262324U (en) * | 2016-10-28 | 2017-06-20 | 浙江海富海洋生物科技有限公司 | One kind ammonia recycle during hydroxyapatite is prepared utilizes device |
-
2016
- 2016-10-28 CN CN201610963447.8A patent/CN106512661A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB730574A (en) * | 1951-05-18 | 1955-05-25 | Kestner App Evaporateurs | Improvements in or relating to the manufacture of diammonium phosphate in pulverulent form |
| CN101249313A (en) * | 2008-04-01 | 2008-08-27 | 南京特种气体厂有限公司 | Recovery cyclic utilization method and apparatus for recovering discharged alkaline air in process of production of silicone hydride with magnesium silicide method |
| CN101607719A (en) * | 2008-06-20 | 2009-12-23 | 南通江山农药化工股份有限公司 | The clean reclaiming process of ammonia gas as byproduct of glyphosate |
| CN101613338A (en) * | 2009-07-21 | 2009-12-30 | 西安交通大学 | A kind of preparation method of cyclic carbonate of while coproduction ammonium hydrogen phosphate |
| CN101773684A (en) * | 2010-03-19 | 2010-07-14 | 西南大学 | Preparation method of fibroin/hydroxyapatite porous scaffold |
| CN202054624U (en) * | 2011-04-28 | 2011-11-30 | 杭州胜大药业有限公司 | Ammonia gas recycling device for nicotinic acid process |
| CN102319534A (en) * | 2011-08-25 | 2012-01-18 | 江西金达莱环保研发中心有限公司 | Method for exhaust gas purification |
| CN202366608U (en) * | 2011-12-20 | 2012-08-08 | 厦门市格绿科技有限公司 | Ammonia recovery device |
| CN203577568U (en) * | 2013-11-27 | 2014-05-07 | 上海众一石化工程有限公司 | Tail gas recycling device |
| CN206262324U (en) * | 2016-10-28 | 2017-06-20 | 浙江海富海洋生物科技有限公司 | One kind ammonia recycle during hydroxyapatite is prepared utilizes device |
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| Title |
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| 胡华锋等: "《畜禽养殖废弃物处理与利用》", 31 August 2016, 中原农民出版社 * |
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