CN102502907A - 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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- CN102502907A CN102502907A CN2011103110334A CN201110311033A CN102502907A CN 102502907 A CN102502907 A CN 102502907A CN 2011103110334 A CN2011103110334 A CN 2011103110334A CN 201110311033 A CN201110311033 A CN 201110311033A CN 102502907 A CN102502907 A CN 102502907A
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- attapulgite
- phosphoric acid
- defluorination
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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 working method of compound defluorination filter bulb, especially a kind of working method that is applicable to the compound defluorination filter bulb of attapulgite load Win 40350 of removing the fluorine that exceeds standard in the tap water.
Background technology
Fluorine is one of the widest element of earth surface distribution, it is generally acknowledged, the fluorine of trace helps the soundness of bone, but excessive fluorine is to toxic elements in human body.Because up to 90%, therefore intravital fluorine is mainly from tap water to the fluorine specific absorption in the tap water for human body.Drink the fluorosis that water of high fluorine content causes and relate to worldwide endemy, the lighter causes dental fluorosis, and weight person can cause skeletal fluorosis.The content of fluorine is no more than 1.5mg/L in World Health Organization's regulation tap water.Because 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, backward in economy, rural area, pastoral area that income is not high; Although therefore the drinking water defluorination technical 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, like 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.Win 40350 has good IX and absorption property as the functional materials of drinking water treatment, and safely, have no side effect, not only can remove excessive fluoride in the tap water, can also remove anhydrate in other harmful elements.At present in the research of Win 40350 defluorinating agent; It is more relatively that hydroxy apatite powder is studied; Like patent of invention number is 200610029366.7 to disclose a kind of preparation method through improved hydroxy apatite powder; This hydroxy apatite powder is prone to harden in the defluorination process, and the water flows resistance is big, is unfavorable for the regeneration of defluorinating agent.Patent of invention number is 201010264616.1 to disclose a kind of working method of drinking water defluoridation filtering material, and this defluoridation filter material is the porous spherical Win 40350, has high, the advantages such as regeneration is prone to, water outlet smoothness of defluorination capacity.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, helps large-scale commercial prodn and applies.But the control of ratio of calcium and phosphorus and pH value in this working method is the key of producing the pure article of Win 40350, if control is bad, is prone in the product mix sub products such as secondary calcium phosphate, monocalcium phosphate, calcium phosphate, influences the defluorination capacity of product.
Summary of the invention
Technical problem: the objective of the invention is to overcome the weak point in the prior art, the working method of the attapulgite load Win 40350 defluorination filter bulb that a kind of preparation technology is simple, easy to control, defluorination filter bulb capacity high, purity is high is provided.
Technical scheme: the working method of the compound defluorination filter bulb of attapulgite load Win 40350 of the present invention:
The preparation of a, attapulgite load hydroxy apatite powder:
(1) adopting calcium hydroxide, phosphoric acid, acetic acid and the attapulgite of technical grade is raw material;
(2) water of adding reaction kettle capacity 50% in reaction kettle is warming up to 75-80 ℃;
(3) in reaction kettle, add a certain amount of acetic acid, stir, the mass percent of a certain amount of acetic acid and water is 0.2～0.4%;
(4) take by weighing the calcium hydroxide that accounts for quality 25%, join in the reaction kettle, stirred 3 ~ 5 minutes;
(5) take by weighing the phosphoric acid of calcium hydroxide quality 80～88%, phosphoric acid is joined 3 times in the water of phosphoric acid volume, be made into phosphoric acid solution;
(6) phosphoric acid solution is added drop-wise in the reaction kettle, rate of addition is 10-15kg/min;
(7) under 75-80 ℃ of temperature, reacted 2.5 hours;
(8) attapulgite of adding calcium hydroxide quality 50-60% stirs, and reaction is 1 hour under 75-80 ℃ of temperature;
(9) take out product, dewater, wash, dry, pulverizing, obtain attapulgite load hydroxy apatite powder;
The preparation of b, attapulgite load Win 40350 defluorination filter bulb:
(1) attapulgite load hydroxy apatite powder is put into nodulizer, the sprinkling mass percent is 1～1.5% Xylo-Mucine or Natvosol tackiness agent, and powder is processed the bead that diameter is 0.5～1.5mm;
(2) take out bead, dryness finalization under 350-450 ° of C, promptly obtaining diameter is the compound defluorination filter bulb of attapulgite load Win 40350 of 0.5-1.5mm.
Beneficial effect: it is raw material that the present invention adopts cheap calcium hydroxide, phosphoric acid, acetic acid and attapulgite; Synthetic attapulgite load Win 40350 ball; Wherein acetic acid plays the solubleness of regulation and control calcium hydroxide; The ratio of calcium and phosphorus in the control solution and the effect of pH value are to guarantee product gas purity and defluorination capacity; Attapulgite and Win 40350 are compound, have reduced cost, help balling-up, simultaneously the Win 40350 defluorination are played synergism.The present invention has that low in raw material cost is easy to get, preparation technology is simple, easy to control, defluorination filter bulb capacity high, regeneration is prone to, the life-span is long, the smooth resistance of water outlet is little, be easy to large-scale commercial prodn and apply.Mainly have the following advantages:
1, the defluorination capacity of product is high, and compared with present technology, the defluorination capacity of product improves 25%;
2, yield of product and purity are high, have reduced the total cost of product;
3, production technique is simple and easy to control, helps scale operation and utilization and extention.
Embodiment
With one ton of reaction kettle is example, technical grade calcium hydroxide content 92%, and phosphorus acid content 85%, acetic acid content are 100%.
Embodiment 1:
1, in reaction kettle, adds 500L water, be heated to 75 ° of C;
2, add 1.5 kg Glacial acetic acid min. 99.5, stir;
3, take by weighing calcium hydroxide 125Kg, join in the reaction kettle, 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 the reaction kettle, the control rate of addition is 12kg/min;
6, under 75 ° of C temperature, reacted 2.5 hours;
7, add the 70kg attapulgite, stir, reaction is 1 hour under 75 ° of C temperature;
8, take out product, dewater, wash, dry, pulverizing, obtain attapulgite load hydroxy apatite powder;
9, attapulgite load hydroxy apatite powder is put into nodulizer, the sprinkling mass percent is 1% Xylo-Mucine tackiness agent, and powder is processed the bead that diameter is 0.5～1.5mm;
10, take out bead, dryness finalization under 400 ° of C, promptly obtaining diameter is the compound defluorination filter bulb of attapulgite load Win 40350 of 0.5-1.5mm.
Embodiment 2:
1, in reaction kettle, adds 500L water, be heated to 75 ° of C;
2, add the 2kg Glacial acetic acid min. 99.5, stir;
3, take by weighing calcium hydroxide 125Kg, join in the reaction kettle, 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 the reaction kettle, the control rate of addition is 10kg/min;
6, under 75 ° of C temperature, reacted 2.5 hours;
7, add the 63kg attapulgite, stir, reaction is 1 hour under 75 ° of C temperature;
8, take out product, dewater, wash, dry, pulverizing, obtain attapulgite load hydroxy apatite powder;
9, attapulgite load hydroxy apatite powder is put into nodulizer, the sprinkling mass percent is 1% Natvosol tackiness agent, and powder is processed the bead that diameter is 0.5～1.5mm;
10, take out bead, dryness finalization under 350 ° of C, promptly obtaining diameter is the compound defluorination filter bulb of attapulgite load Win 40350 of 0.5-1.5mm.
Embodiment 3:
1, in reaction kettle, adds 500L water, be heated to 80 ° of C;
2, add the 1kg Glacial acetic acid min. 99.5, stir;
3, take by weighing calcium hydroxide 125Kg, join in the reaction kettle, 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 the reaction kettle, the control rate of addition is 15kg/min;
6, under 80 ° of C temperature, reacted 2.5 hours;
7, add the 75kg attapulgite, stir, reaction is 1 hour under 80 ° of C temperature;
8, take out product, dewater, wash, dry, pulverizing, obtain attapulgite load hydroxy apatite powder;
9, attapulgite load hydroxy apatite powder is put into nodulizer, the sprinkling mass percent is 1.5% Xylo-Mucine tackiness agent, and powder is processed the bead that diameter is 0.5～1.5mm;
10, take out bead, dryness finalization under 450 ° of C, promptly obtaining diameter is the compound defluorination filter bulb of attapulgite load Win 40350 of 0.5-1.5mm.
Claims (1)
1. the working method of the compound defluorination filter bulb of attapulgite load Win 40350 is characterized in that comprising the steps:
The preparation of a, attapulgite load hydroxy apatite powder:
(1) adopting calcium hydroxide, phosphoric acid, acetic acid and the attapulgite of technical grade is raw material;
(2) water of adding reaction kettle capacity 50% in reaction kettle is warming up to 75-80 ℃;
(3) in reaction kettle, add a certain amount of acetic acid, stir, the mass percent of a certain amount of acetic acid and water is 0.2～0.4%;
(4) take by weighing the calcium hydroxide that accounts for quality 25%, join in the reaction kettle, stirred 3 ~ 5 minutes;
(5) take by weighing the phosphoric acid of calcium hydroxide quality 80～88%, phosphoric acid is joined 3 times in the water of phosphoric acid volume, be made into phosphoric acid solution;
(6) phosphoric acid solution is added drop-wise in the reaction kettle, rate of addition is 10-15kg/min;
(7) under 75-80 ℃ of temperature, reacted 2.5 hours;
(8) attapulgite of adding calcium hydroxide quality 50-60% stirs, and reaction is 1 hour under 75-80 ℃ of temperature;
(9) take out product, dewater, wash, dry, pulverizing, obtain attapulgite load hydroxy apatite powder;
The preparation of b, attapulgite load Win 40350 defluorination filter bulb:
(1) attapulgite load hydroxy apatite powder is put into nodulizer, the sprinkling mass percent is 1～1.5% Xylo-Mucine or Natvosol tackiness agent, and powder is processed the bead that diameter is 0.5～1.5mm;
(2) take out bead, dryness finalization under 350-450 ° of C, promptly obtaining diameter is the compound defluorination filter bulb of attapulgite load Win 40350 of 0.5-1.5mm.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104193028A (en) * | 2014-06-16 | 2014-12-10 | 江苏永冠给排水设备有限公司 | Fluorine removal method for compound drinking water |
| CN106745364A (en) * | 2016-11-30 | 2017-05-31 | 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 |
| CN110038510A (en) * | 2019-04-29 | 2019-07-23 | 南京大学 | A kind of preparation method of the modified calcite adsorbent of 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 |
| CN111514846A (en) * | 2020-04-20 | 2020-08-11 | 西安斯威夫特环保科技有限公司 | Preparation method of defluorination filter material |
| WO2022088309A1 (en) * | 2020-10-27 | 2022-05-05 | 南京长三角绿色发展研究院有限公司 | Biomass-based hydroxyapatite composite material, preparation method therefor and application thereof |
| CN115779856A (en) * | 2022-11-21 | 2023-03-14 | 煤炭科学技术研究院有限公司 | Hydroxyapatite/active carbon composite defluorination material and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104193028A (en) * | 2014-06-16 | 2014-12-10 | 江苏永冠给排水设备有限公司 | Fluorine removal method for compound drinking water |
| CN106745364A (en) * | 2016-11-30 | 2017-05-31 | 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 |
| CN110038510A (en) * | 2019-04-29 | 2019-07-23 | 南京大学 | A kind of preparation method of the modified calcite adsorbent of 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 |
| CN111514846A (en) * | 2020-04-20 | 2020-08-11 | 西安斯威夫特环保科技有限公司 | Preparation method of defluorination filter material |
| WO2022088309A1 (en) * | 2020-10-27 | 2022-05-05 | 南京长三角绿色发展研究院有限公司 | Biomass-based hydroxyapatite composite material, preparation method therefor and application thereof |
| CN115779856A (en) * | 2022-11-21 | 2023-03-14 | 煤炭科学技术研究院有限公司 | Hydroxyapatite/active carbon composite defluorination material and preparation method thereof |
| CN115779856B (en) * | 2022-11-21 | 2024-05-07 | 煤炭科学技术研究院有限公司 | Hydroxyapatite/activated carbon composite defluorination material and preparation method thereof |
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