CN102502907B - Production method of attapulgite loaded hydroxyapatite composite defluorination filter bulb - Google Patents
Production method of attapulgite loaded hydroxyapatite composite defluorination filter bulb Download PDFInfo
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- CN102502907B CN102502907B CN 201110311033 CN201110311033A CN102502907B CN 102502907 B CN102502907 B CN 102502907B CN 201110311033 CN201110311033 CN 201110311033 CN 201110311033 A CN201110311033 A CN 201110311033A CN 102502907 B CN102502907 B CN 102502907B
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Abstract
The invention discloses a production method of an attapulgite loaded hydroxyapatite composite defluorination filter bulb, which comprises the following steps: preparing attapulgite loaded hydroxyapatite powder from industrial-grade calcium hydroxide, phosphoric acid, acetic acid and attapulgite as raw materials, regulating the solubility of calcium hydroxide using acetic acid, and controlling calcium-phosphorus ratio and pH value of the solution so as to ensure the purity and the defluorination capacity of the products; and fabricating the attapulgite loaded hydroxyapatite powder into pellets of diameters 0.5-1.5mm, and drying and molding the pellets at a temperature ranging from 350 to 450 DEG C so as to obtain attapulgite loaded hydroxyapatite composite defluorination filter bulb. The composition of attapulgite and hydroxyapatite reduces cost, is helpful for pellet formation, and enhances defluorination of hydroxyapatite. The method of the invention uses cheap and easily-accessible raw materials, high capacity of defluorination filter bulbs, long service life and small fluent water resistance, , and is simple in preparation, easy for control and regeneration, and easy for large-scale industrial production and promotion.
Description
Technical field
The present invention relates to a kind of production method of composite defluorination filter bulb, especially a kind ofly be applicable to remove the production method of attapulgite loaded hydroxyapatite composite defluorination filter bulb of fluorine of exceeding standard in tap water.
Background technology
Fluorine is one of the widest element of earth surface distribution, it is generally acknowledged, the fluorine of trace is conducive to the soundness of bone, but excessive fluorine is poisonous to human body.Due to human body to the fluorine specific absorption in tap water up to 90%, so body in fluorine mainly from tap water.Drink the fluorosis that water of high fluorine content causes and relate to worldwide endemy, the lighter causes dental fluorosis, and severe one can cause skeletal fluorosis.In World Health Organization's regulation tap water, the content of fluorine is no more than 1.5mg/L.Due to water of high fluorine content is distributed in mainly that environment is abominable, with a varied topography, the few electricity of lack of water, have inconvenient traffic, rural area, the pastoral area that backward in economy, income is not high, although therefore the developing tendency of removal of fluoride from drinking development is very fast, absorption method remains at present the most frequently used drinking water defluorination method both at home and abroad.The de-fluoridation adsorbent kind is more, as zeolite, clay, gac, activated alumina and bone carbon etc., but considers difficulty or ease, cost and the defluorination capacity of renovation process, and many sorbent materials do not obtain practical application.
Attapulgite is a kind of moisture zeopan sodium crystal mineral, has certain absorption property owing to having unique crystalline structure, but single use attapulgite is as sorbent material, and its absorption property and adsorption effect have certain limitation.Hydroxyapatite has good ion-exchange and absorption property as the functional materials of drinking water treatment, and safely, have no side effect, not only can remove excessive fluoride in tap water, can also be except other harmful elements in anhydrating.At present in the research of hydroxyapatite defluorinating agent, it is relatively many that hydroxy apatite powder is studied, number be 200610029366.7 to disclose a kind of preparation method through improved hydroxy apatite powder as patent of invention, this hydroxy apatite powder easily hardens in the defluorination process, the water flow resistance is large, is unfavorable for the regeneration of defluorinating agent.Patent of invention number is 201010264616.1 to disclose a kind of production method of drinking water defluoridation filtering material, and this defluoridation filter material is the porous spherical hydroxyapatite, have that the defluorination capacity is high, regeneration easily, the advantage such as water outlet is smooth.Wherein hydroxy apatite powder adopts cheap raw material, utilizes the precipitator method synthetic, and production technique is simple and easy to control, facility investment is low, is conducive to large-scale commercial production and applies.But the control of ratio of calcium and phosphorus and pH value in this production method is the key of producing the hydroxyapatite sterling, if control badly, easily mixes the byproducts such as secondary calcium phosphate, monocalcium phosphate, calcium phosphate in product, affects the defluorination capacity of product.
Summary of the invention
Technical problem: the objective of the invention is to overcome the weak point in prior art, the production method of the attapulgite loaded hydroxyapatite defluorination filter bulb that a kind of preparation technology is simple, easy to control, the defluorination filter bulb capacity is high, purity is high is provided.
Technical scheme: the production method of attapulgite loaded hydroxyapatite composite defluorination filter bulb of the present invention:
The preparation of a, attapulgite loaded hydroxyapatite powder:
(1) adopting calcium hydroxide, phosphoric acid, acetic acid and the attapulgite of technical grade is raw material;
(2) add the water of reactor capacity 50% in reactor, be warming up to 75-80 ℃;
(3) add a certain amount of acetic acid in reactor, stir, the mass percent of a certain amount of acetic acid and water is 0.2～0.4%;
(4) take the calcium hydroxide that accounts for quality 25%, join in reactor, stirred 3 ~ 5 minutes;
(5) take the phosphoric acid of calcium hydroxide quality 80～88%, phosphoric acid is joined 3 times be made into phosphoric acid solution in the water of phosphoric acid volume;
(6) phosphoric acid solution is added drop-wise in reactor, rate of addition is 10-15kg/min;
(7) reacted 2.5 hours at 75-80 ℃ of temperature;
(8) add the attapulgite of calcium hydroxide quality 50-60%, stir, reaction is 1 hour at 75-80 ℃ of temperature;
(9) take out product, dewater, wash, dry, pulverizing, obtain the attapulgite loaded hydroxyapatite powder;
The preparation of b, attapulgite loaded hydroxyapatite defluorination filter bulb:
(1) the attapulgite loaded hydroxyapatite powder is put into nodulizer, the sprinkling mass percent is 1～1.5% Xylo-Mucine or Natvosol tackiness agent, and powder is made the bead that diameter is 0.5～1.5mm;
(2) take out bead, dryness finalization under 350-450 ° of C namely obtains the attapulgite loaded hydroxyapatite composite defluorination filter bulb that diameter is 0.5-1.5mm.
Beneficial effect: it is raw material that the present invention adopts cheap calcium oxide, phosphoric acid, acetic acid and attapulgite, synthetic attapulgite loaded hydroxyapatite ball, wherein acetic acid plays the solubleness of regulation and control calcium hydroxide, ratio of calcium and phosphorus in control solution and the effect of pH value are to guarantee purity and the defluorination capacity of product; Attapulgite and hydroxyapatite are compound, have reduced cost, are conducive to balling-up, simultaneously the hydroxyapatite defluorination are played synergism.The present invention has that raw material is cheap and easy to get, preparation technology is simple, easy to control, the defluorination filter bulb capacity is high, regeneration easily, the life-span is long, the smooth resistance of water outlet is little, be easy to large-scale commercial production and apply.Mainly have the following advantages:
1, the defluorination capacity of product is high, and compared with the prior art, the defluorination capacity of product improves 25%;
2, the productive rate of product and purity are high, have reduced the total cost of product;
3, production technique is simple and easy to control, is conducive to scale operation and utilization and extention.
Embodiment
Take one ton of reactor as example, technical grade calcium hydroxide content 92%, phosphorus acid content 85%, acetic acid content are 100%.
Embodiment 1:
1, add 500L water in reactor, be heated to 75 ° of C;
2, add 1.5 kg Glacial acetic acid, stir;
3, take calcium hydroxide 125Kg, join in reactor, stirred 4 minutes;
4,105kg phosphoric acid is added the wiring solution-forming that stirs in the water of 315kg;
5, above-mentioned phosphoric acid solution is added drop-wise in reactor, the control rate of addition is 12kg/min;
6, reacted 2.5 hours at 75 ° of C temperature;
7, add the 70kg attapulgite, stir, reaction is 1 hour at 75 ° of C temperature;
8, take out product, dewater, wash, dry, pulverizing, obtain the attapulgite loaded hydroxyapatite powder;
9, the attapulgite loaded hydroxyapatite powder is put into nodulizer, the sprinkling mass percent is 1% Xylo-Mucine tackiness agent, and powder is made the bead that diameter is 0.5～1.5mm;
10, take out bead, dryness finalization under 400 ° of C namely obtains the attapulgite loaded hydroxyapatite composite defluorination filter bulb that diameter is 0.5-1.5mm.
Embodiment 2:
1, add 500L water in reactor, be heated to 75 ° of C;
2, add the 2kg Glacial acetic acid, stir;
3, take calcium hydroxide 125Kg, join in reactor, stirred 5 minutes;
4,100kg phosphoric acid is added the wiring solution-forming that stirs in the water of 300kg;
5, above-mentioned phosphoric acid solution is added drop-wise in reactor, the control rate of addition is 10kg/min;
6, reacted 2.5 hours at 75 ° of C temperature;
7, add the 63kg attapulgite, stir, reaction is 1 hour at 75 ° of C temperature;
8, take out product, dewater, wash, dry, pulverizing, obtain the attapulgite loaded hydroxyapatite powder;
9, the attapulgite loaded hydroxyapatite powder is put into nodulizer, the sprinkling mass percent is 1% Natvosol tackiness agent, and powder is made the bead that diameter is 0.5～1.5mm;
10, take out bead, dryness finalization under 350 ° of C namely obtains the attapulgite loaded hydroxyapatite composite defluorination filter bulb that diameter is 0.5-1.5mm.
Embodiment 3:
1, add 500L water in reactor, be heated to 80 ° of C;
2, add the 1kg Glacial acetic acid, stir;
3, take calcium hydroxide 125Kg, join in reactor, stirred 3 minutes;
4,110kg phosphoric acid is added the wiring solution-forming that stirs in the water of 330kg;
5, above-mentioned phosphoric acid solution is added drop-wise in reactor, the control rate of addition is 15kg/min;
6, reacted 2.5 hours at 80 ° of C temperature;
7, add the 75kg attapulgite, stir, reaction is 1 hour at 80 ° of C temperature;
8, take out product, dewater, wash, dry, pulverizing, obtain the attapulgite loaded hydroxyapatite powder;
9, the attapulgite loaded hydroxyapatite powder is put into nodulizer, the sprinkling mass percent is 1.5% Xylo-Mucine tackiness agent, and powder is made the bead that diameter is 0.5～1.5mm;
10, take out bead, dryness finalization under 450 ° of C namely obtains the attapulgite loaded hydroxyapatite composite defluorination filter bulb that diameter is 0.5-1.5mm.
Claims (1)
1. the production method of attapulgite loaded hydroxyapatite composite defluorination filter bulb, is characterized in that comprising the steps:
The preparation of a, attapulgite loaded hydroxyapatite powder:
(1) adopting calcium hydroxide, phosphoric acid, acetic acid and the attapulgite of technical grade is raw material;
(2) add the water of reactor capacity 50% in reactor, be warming up to 75-80 ℃;
(3) add a certain amount of acetic acid in reactor, stir, the mass percent of a certain amount of acetic acid and water is 0.2～0.4%;
(4) take the calcium hydroxide that accounts for quality 25%, join in reactor, stirred 3 ~ 5 minutes;
(5) take the phosphoric acid of calcium hydroxide quality 80～88%, phosphoric acid is joined 3 times be made into phosphoric acid solution in the water of phosphoric acid volume;
(6) phosphoric acid solution is added drop-wise in reactor, rate of addition is 10-15kg/min;
(7) reacted 2.5 hours at 75-80 ℃ of temperature;
(8) add the attapulgite of calcium hydroxide quality 50-60%, stir, reaction is 1 hour at 75-80 ℃ of temperature;
(9) take out product, dewater, wash, dry, pulverizing, obtain the attapulgite loaded hydroxyapatite powder;
The preparation of b, attapulgite loaded hydroxyapatite defluorination filter bulb:
(1) the attapulgite loaded hydroxyapatite powder is put into nodulizer, the sprinkling mass percent is 1～1.5% Xylo-Mucine or Natvosol tackiness agent, and powder is made the bead that diameter is 0.5～1.5mm;
(2) take out bead, dryness finalization under 350-450 ° of C namely obtains the attapulgite loaded hydroxyapatite composite defluorination filter bulb that diameter is 0.5-1.5mm.
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Families Citing this family (8)
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| CN103725883A (en) * | 2013-12-13 | 2014-04-16 | 来宾华锡冶炼有限公司 | Method for preparing zinc sulfate solution de-fluorination agent |
| CN104193028B (en) * | 2014-06-16 | 2016-02-17 | 江苏永冠给排水设备有限公司 | A kind of compound drinking water defluorination method |
| CN106745364B (en) * | 2016-11-30 | 2018-02-09 | 江苏永冠给排水设备有限公司 | A kind of Implant hydroxyapatite filter grain based on planting method fluorine removal water process and preparation method thereof |
| CN108479693A (en) * | 2018-05-04 | 2018-09-04 | 成都理工大学 | Hydroxyapatite attapulgite composite material and its preparation method and application |
| CN110038510B (en) * | 2019-04-29 | 2020-12-04 | 南京大学 | Preparation method of modified calcite adsorbent for fluorine removal |
| CN110252261A (en) * | 2019-06-21 | 2019-09-20 | 南京信息工程大学 | A kind of resin-base nano hydroxyapatite composite material, preparation method and the application in the processing of fluoride pollution water body |
| CN111514846B (en) * | 2020-04-20 | 2022-12-20 | 西安斯威夫特环保科技有限公司 | Preparation method of defluorination filter material |
| CN112547021A (en) * | 2020-10-27 | 2021-03-26 | 南京长三角绿色发展研究院有限公司 | Biomass-based hydroxyapatite composite material and preparation method and application thereof |
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| CN101343055A (en) * | 2008-08-19 | 2009-01-14 | 华南理工大学 | Nano-hydroxyapatite hydrosol, preparation and application in toothpaste |
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