CN108030947B - A kind of preparation method of modified negative oxygen ion powder - Google Patents

A kind of preparation method of modified negative oxygen ion powder Download PDF

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Publication number
CN108030947B
CN108030947B CN201711261225.2A CN201711261225A CN108030947B CN 108030947 B CN108030947 B CN 108030947B CN 201711261225 A CN201711261225 A CN 201711261225A CN 108030947 B CN108030947 B CN 108030947B
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ion powder
oxygen ion
negative oxygen
ammonium sulfate
solution
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CN108030947A (en
Inventor
于泱
乔文涛
唐卫
曹晓检
闫崇峰
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Shandong Shengyuan Huacheng nano material Co.,Ltd.
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Heilongjiang Lisheng Silicon Nano Materials Science & Technology Development Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L9/00Disinfection, sterilisation or deodorisation of air
    • A61L9/16Disinfection, sterilisation or deodorisation of air using physical phenomena
    • A61L9/22Ionisation
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61NELECTROTHERAPY; MAGNETOTHERAPY; RADIATION THERAPY; ULTRASOUND THERAPY
    • A61N1/00Electrotherapy; Circuits therefor
    • A61N1/44Applying ionised fluids
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage

Abstract

The invention discloses a kind of preparation methods of modified negative oxygen ion powder, belong to chemical technology field, solving existing negative oxygen ion powder has highly polar and particle imperceptibility, be not easy to disperse the problems such as apparent characteristic is bad, laterally irradiation is higher in apolar substance, should the preparation method comprises the following steps: one, prepare ammonium sulfate, barium chloride solution and EDTA solution respectively;Two, under stirring condition, EDTA solution is poured into barium chloride solution;Three, above-mentioned mixed solution is added in negative oxygen ion powder, is uniformly mixed;Four, ammonium sulfate is added dropwise, accelerates stirring a period of time;Five, centrifuge washing is distinguished with deionized water, ethyl alcohol after standing, and is then dried to obtain the negative oxygen ion powder of load nano barium sulfate particle.Preparation method of the present invention is simple, and novel and unique is environmentally friendly, the existing original characteristic of obtained modified negative-ion powder, and combines the characteristic of nano barium sulfate particle, improves the utility value and application field of negative oxygen ion powder.

Description

A kind of preparation method of modified negative oxygen ion powder
Technical field
The present invention relates to a kind of preparation methods of modified negative oxygen ion powder, belong to chemical technology field.
Background technique
Anion is to be present in environment for human survival --- a kind of electronegative ion or ion cluster in atmosphere.It is relied on All multimodes such as air collision, thunder and lightning, radiation, water impact, photosynthesis of plant, substance point discharge generate, to people Class health, living environment quality have very big benefit.Therefore, negative aeroion enjoys " tie up his oxygen ", " air in medical field The laudatory titles such as vitamin ", " long-lived element ", " air vitamin ", and measure one of the important indicator of air cleaner degree.Anion Research it is significant to human health and living environment, to the effect of human health be mainly reflected in respiration health, promote blood Liquid circulation adjusts human body ionic equilibrium and inhibits fungus attack etc., and to the effect of environment be mainly reflected in purification air, Purify water in bactericidal effect.Closely bound up, the Ren Menyue just because of anion concentration in living environment and our existence More to pay attention to the research to anion related content.
Negative ion powder is that multiple element mixes, and ingredient has pyroelectricity and piezoelectricity, is there is temperature and pressure change It can cause the potential difference between negative ion powder crystal in the case where change, so that air is ionized, the electron attachment hit In on neighbouring hydrone or oxygen molecule and it being made to be converted into anion.Negative ion powder has highly polar and particle subtle Change, be not easy to disperse in apolar substance that apparent characteristic is bad, laterally irradiation is higher, is not only difficult to and properties of product It is corresponding to reduce.
Summary of the invention
The purpose of the invention is to improve the problem that negative oxygen ion powder apparent characteristic is bad, lateral irradiation is higher, and mention For a kind of preparation method with the particle modified negative oxygen ion powder of nano barium sulfate with microwave absorbing property, to expand its application Advantage and range.
The preparation method of the modified negative oxygen ion powder of the present invention follows these steps to realize:
One, ammonium sulfate, barium chloride solution and EDTA solution are prepared respectively;
Two, under the conditions of being stirred at room temperature, EDTA solution is poured into barium chloride solution, regulation system pH is 6~8, stirring, Obtain mixed liquor A;
Three, negative oxygen ion powder is taken, above-mentioned mixed liquor A is added under stirring condition, is uniformly mixed and obtains mixed liquid B;
Four, ammonium sulfate is added dropwise into mixed liquid B, stirs;
Five, the mixture that step 4 obtains is stood, and is centrifuged to obtain precipitating, successively distinguishes centrifuge washing 3 with deionized water, ethyl alcohol ~5 times, gained precipitating is dried to obtain the modification negative oxygen ion powder of load nano barium sulfate particle.
Preferably, it is (5- that the ratio between the EDTA of mixed liquor A and the amount of substance of barium chloride are used to prepare described in step 2 kind 6):(5-6)。
Preferably, the substance of EDTA used in the ammonium sulfate and step 2 that step 4 kind is added dropwise in ammonium sulfate The ratio between amount is (5-6): (5-6).
Preferably, in step 3 EDTA used in negative oxygen ion powder and step 2 quality (g), the amount of substance (mmol) Than for (5.8-11.6): (25-30).
Preferably, the concentration of three kinds of solution described in step 1 is 0.5mol/L.
Preferably, the temperature condition of step 2 operation is 22~27 DEG C of room temperature, and ammonia water conditioning system pH is used in step 2, The stirring after adjusting pH step, mixing time are 20~30min.
Preferably, negative oxygen ion powder described in step 3 is commercially available negative oxygen ion powder;It is described be uniformly mixed, by stirring 5~ 8min is realized.
Preferably, ammonium sulfate rate of addition described in step 4 is 10~50mL/min;The stirring, speed compared with The mixing speed of step 3 kind accelerates 30~50rpm, and mixing time is 30~40min.
Preferably, dry described in step 5, temperature is 55~65 DEG C;The standing, time are 3~4h.
Rapid one uses ammonium sulfate and barium chloride as the presoma for forming nano barium sulfate particle.
It is complexing agent that EDTA is used in step 1.
The present invention makes it load nanoscale using barium chloride as presoma using the modified negative oxygen ion powder of EDTA complexometry Barium sulfate particles.This method novel and unique, easy to operate, process safety is reliable and environmentally friendly, both combines negative oxygen ion The two-fold advantage of powder and nano barium sulfate particle, and negative oxygen ion powder existing deficiency in terms of radiation is improved, optimize simultaneously Apparent characteristic dispersibility is improved, to expand the application range of negative oxygen ion powder, greatly improves its benefit With value.
Detailed description of the invention
Fig. 1 is the schematic diagram of the method for the present invention;
Fig. 2 is the digital photograph that embodiment one reacts front and back negative oxygen ion powder;
Fig. 3 is the radiation curve that embodiment one reacts front and back negative oxygen ion powder.
Specific embodiment
Specific embodiment one: the preparation method of the modified negative oxygen ion powder of present embodiment follows these steps to implement:
One, ammonium sulfate, barium chloride solution and each 50~60mL of EDTA solution of 0.5mol/L are prepared respectively;
Two, under the conditions of being stirred at room temperature, 50~60mL EDTA solution is poured into 50~60mL barium chloride solution, ammonium hydroxide 20~30min is stirred in regulation system PH=6~8;
Three, 500mL there-necked flask is separately taken, 5.8~11.6g negative oxygen ion powder is added, it is molten that above-mentioned mixing is added under stirring condition Liquid, 5~8min of stirring is so that it is uniformly mixed;
Four, 50~60mL ammonium sulfate is added dropwise, accelerates stirring, stirs 30~40min;
Five, distinguished centrifuge washing 3~5 times after standing with deionized water, ethyl alcohol, it is then dry in 55~65 DEG C of baking ovens To the negative oxygen ion powder of load nano barium sulfate particle.
Area load nanoscale barium sulfate grain can be obtained using the preparation method of the modified negative oxygen ion powder of present embodiment The negative oxygen ion powder of son.Ammonium sulfate is added dropwise in step 4 and uses dropping funel or syringe pump, rate of addition 10mL/ min。
Specific embodiment 2: the present embodiment is different from the first embodiment in that the temperature of step 2 is 45 DEG C. Other steps and parameter are same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that system PH is in step 2 8~10, other steps and parameter are the same as one or two specific embodiments.
Specific embodiment 4: negative oxygen in step 3 unlike one of present embodiment and specific embodiment one to three Ion powder additive amount is 11.6~17.5g.Other steps and parameter are identical as one of specific embodiment one to three.
Embodiment one: the preparation method of the modified negative oxygen ion powder of the present embodiment follows these steps to implement:
One, ammonium sulfate, barium chloride solution and each 50mL of EDTA solution of 0.5mol/L are prepared respectively;
Two, 50mL EDTA solution is poured into 50mL barium chloride solution under the conditions of 25 DEG C of room temperature, ammonia water conditioning system PH =6, stirring 20min obtains mixed liquor A;
Three, 500mL there-necked flask is separately taken, 11.6g negative oxygen ion powder is added, above-mentioned mixed liquor A is added under stirring condition, stirs 5min obtains mixed liquid B so that it is uniformly mixed;
Four, 50mL ammonium sulfate is added dropwise to mixed liquid B with the speed of 10mL/min using dropping funel, accelerates stirring, Mixing speed accelerates 30rpm compared with the mixing speed of step 3 kind, stirs 30min;
Five, it is centrifuged after standing 3h, must precipitate and successively be distinguished centrifuge washing 3 times with deionized water, ethyl alcohol, then be dried at 60 DEG C The negative oxygen ion powder of load nano barium sulfate particle is dried to obtain in case.
Obtained negative oxygen ion powder is dispersed in n-hexane, is uniformly dispersed.Fig. 2 be the reaction of the embodiment one negative oxygen in front and back from The digital photograph of sub- powder, khaki negative oxygen ion powder becomes after loading nano barium sulfate particle before as can be seen from the figure reacting For white powder, finer and smoother state is apparently showed;Fig. 3 is the radiation song that embodiment one reacts front and back negative oxygen ion powder Line, as can be seen from the figure External Exposure Index and Outreach services are above national normal value to negative oxygen ion powder before treatment, and The External Exposure Index and Outreach services of negative oxygen ion powder in load after nano barium sulfate particle are below national normal value, greatly It is improved greatly in the application value in the higher field of environmental requirement.
Embodiment two
One, ammonium sulfate, barium chloride solution and each 60mL of EDTA solution of 0.5mol/L are prepared respectively;
Two, under 22 DEG C of stirring conditions, 60mL EDTA solution is poured into 50mL barium chloride solution, ammonia water conditioning system PH=6, stirring 20min obtain mixed liquor A;
Three, 500mL there-necked flask is separately taken, the commercially available negative oxygen ion powder of 5.8g is added, above-mentioned mixed liquor A is added under stirring condition, It stirs
5min is mixed so that it, which is uniformly mixed, obtains mixed liquid B;
Four, 50mL ammonium sulfate is added dropwise to mixed liquid B with the speed of 10mL/min using syringe pump, accelerates stirring, stirs The mixing speed that speed is mixed compared with step 3 kind accelerates 30rpm, stirs 30min;
Five, the mixture that step 4 obtains is centrifuged after standing 3h, must be precipitated successively to be centrifuged respectively with deionized water, ethyl alcohol and be washed It washs 3 times, the negative oxygen ion powder of load nano barium sulfate particle is then dried to obtain in 55 DEG C of baking ovens.
Embodiment three
One, ammonium sulfate, barium chloride solution and each 60mL of EDTA solution of 0.5mol/L are prepared respectively;
Two, under 27 DEG C of stirring conditions, 60mL EDTA solution is poured into 50mL barium chloride solution, ammonia water conditioning system PH=8, stirring 30min obtain mixed liquor A;
Three, 500mL there-necked flask is separately taken, the commercially available negative oxygen ion powder of 11.6g is added, above-mentioned mixed liquor A is added under stirring condition,
Stirring 8min obtains mixed liquid B so that it is uniformly mixed;
Four, 60mL ammonium sulfate is added dropwise to mixed liquid B with the speed of 50mL/min using syringe pump, accelerates stirring, stirs The mixing speed that speed is mixed compared with step 3 kind accelerates 50rpm, stirs 40min;
Five, the mixture that step 4 obtains is centrifuged after standing 4h, must be precipitated successively to be centrifuged respectively with deionized water, ethyl alcohol and be washed It washs 5 times, the negative oxygen ion powder of load nano barium sulfate particle is then dried to obtain in 65 DEG C of baking ovens.

Claims (1)

1. a kind of preparation method of modified negative oxygen ion powder, it is characterised in that: be to follow these steps to realize:
One, ammonium sulfate, barium chloride solution and EDTA solution are prepared respectively;
Two, under the conditions of being stirred at room temperature, EDTA solution is poured into barium chloride solution, regulation system pH is 6~8, stirring,
Obtain mixed liquor A;
Three, negative oxygen ion powder is taken, above-mentioned mixed liquor A is added under stirring condition, is uniformly mixed and obtains mixed liquid B;
Four, ammonium sulfate is added dropwise into mixed liquid B, stirs;
Five, the mixture that step 4 obtains is stood, and is centrifugated to obtain precipitating, successively distinguishes centrifuge washing 3 with deionized water, ethyl alcohol ~5 times, gained precipitating is dried to obtain the modification negative oxygen ion powder of load nano barium sulfate particle;
It is (5-6): (5-6) that the ratio between the EDTA of mixed liquor A and the amount of substance of barium chloride are used to prepare described in step 2;Step The ratio between amount of substance of EDTA used in the ammonium sulfate in ammonium sulfate and step 2 being added dropwise in four is (5-6): (5- 6);The mass volume ratio of negative oxygen ion powder and EDTA used in step 2 are (5.8-11.6): (50-60) g/ in step 3 mL;The concentration of three kinds of solution described in step 1 is 0.5mol/L;Negative oxygen ion powder described in step 3 is commercially available negative oxygen ion powder; It is described to be uniformly mixed, it is realized by 5~8min of stirring;The temperature condition of step 2 operation is 22~27 DEG C of room temperature, in step 2 Using ammonia water conditioning system pH, the stirring after pH step is adjusted, mixing time is 20~30min;Sulphur described in step 4 Acid ammonium solution rate of addition is 10~50mL/min;It is stirred described in step 4, speed is accelerated compared with the mixing speed in step 3 30~50rpm, mixing time are 30~40min;Dry described in step 5, temperature is 55~65 DEG C;The standing, time is 3~4h.
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CN114592379A (en) * 2022-03-16 2022-06-07 齐鲁工业大学 Negative oxygen ion coating for coating in machine and light offset paper

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101145703B1 (en) * 2010-11-24 2012-05-24 (주)에나인더스트리 Radiation shield sheet
CN102863003A (en) * 2012-09-26 2013-01-09 中国科学院宁波材料技术与工程研究所 In-site controllable synthetic method for surface modified nano barium sulfate powder
CN107325625A (en) * 2017-08-16 2017-11-07 河北卓达建材研究院有限公司 A kind of negative ion powder and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101145703B1 (en) * 2010-11-24 2012-05-24 (주)에나인더스트리 Radiation shield sheet
CN102863003A (en) * 2012-09-26 2013-01-09 中国科学院宁波材料技术与工程研究所 In-site controllable synthetic method for surface modified nano barium sulfate powder
CN107325625A (en) * 2017-08-16 2017-11-07 河北卓达建材研究院有限公司 A kind of negative ion powder and preparation method thereof

Non-Patent Citations (1)

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Title
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Address before: 150028 room 2, unit 1, 1, business accelerator Park, 15255 Zhong Yuan Road, Harbin, Heilongjiang.

Patentee before: HEILONGJIANG LISHENG NANO SILICON MATERIAL TECHNOLOGY DEVELOPMENT Co.,Ltd.

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