CN105126782B - Based on diatomaceous granular filter material and its preparation method and application - Google Patents

Based on diatomaceous granular filter material and its preparation method and application Download PDF

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CN105126782B
CN105126782B CN201510464955.7A CN201510464955A CN105126782B CN 105126782 B CN105126782 B CN 105126782B CN 201510464955 A CN201510464955 A CN 201510464955A CN 105126782 B CN105126782 B CN 105126782B
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kieselguhr
steaming
decocting
filter material
diatomaceous
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CN105126782A (en
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文启东
崔俊峰
邹晓虎
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INNER MONGOLIA DONGSHENG DIATOMITE TECHNOLOGY INNOVATION INDUSTRIAL PARK CO., LTD.
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Inner Mongolia Dongsheng Diatomite Technology Innovation Industrial Park Co Ltd
Beijing Dongtai Fubo New Material Science & Technology Co Ltd
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Abstract

The invention provides a kind of for preparation method based on diatomaceous granular filter material, it is characterised in that described method mainly comprises the steps: to obtain diatomite powder;By described diatomite powder and monoacidic base aqueous solution steaming and decocting, it is thus achieved that kieselguhr cooking liquor;Described kieselguhr cooking liquor is filtered, it is thus achieved that kieselguhr steaming and decocting filtrate;Add glycerol, polyvinylpyrrolidone and ethanol to described kieselguhr steaming and decocting filtrate successively and stir;By pH regulator to pH 5 to 6, then stand to gelling in room temperature, obtain the first kieselguhr gel;By described first kieselguhr soak 12 hours to 18 hours in ethanol, obtain the second kieselguhr gel;Described second kieselguhr gel is carried out supercritical drying, obtains described based on diatomaceous granular filter material.By the ability with significantly absorption formaldehyde of the granular filter material obtained by the method for the present invention, may be used for indoor air filtration, such as, can be made into filter element and be put in the air channel of air conditioner.

Description

Based on diatomaceous granular filter material and its preparation method and application
Technical field
The present invention relates to the preparation of filtering material
Background technology
The molecular formula of formaldehyde is HCHO, and molecular weight is 30.03, is simplest aldehydes, normal conditions Under be gas a kind of flammable, colourless and excitatory.Formaldehyde is a kind of important Organic Ingredients, mainly For plastics industry (such as phenolic resin processed, urea-formaldehyde plastics), synthetic fibers (such as synthesis vinylon polyvinyl alcohol Formal), leather industry, medicine, dyestuff etc..But, formaldehyde has obvious toxicity.People sucks 60~120mg/m3, occur bronchitis, pulmonary seriously to damage;People sucks 12~24mg/m3, nose, Pharyngeal mucous membrane third-degree burn, shed tears, cough;People's per os 10~20ml is lethal.People sucks 20~70mg/m3 For a long time, loss of appetite, lose weight, unable, have a headache, have a sleepless night;People sucks 12mg/m3Connect for a long time Touch, drowsiness, unable, headache, finger tremble, visual deterioration.Mammalian somatic cell suddenlys change: people is drenched Bar cell 130 μm ol/L;But also reproductive system may be produced harmful effect, and may cause Cancer.It is reported, formaldehyde has intense stimulus to eyes, respiratory tract and skin.Formaldehyde Exposed steam draws Play conjunctivitis, keratitis, rhinitis or bronchitis, thus may cause laryngospasm, glottic edema, lung Scorching, pulmonary edema.It addition, skin is had constitutional to stimulate and sensitization by formaldehyde.Dermatitis can be caused.Dense molten Liquid can cause skin coagulation necrosis.Oral burn oral cavity and digestive tract, can occur gastrointestinal perforation, stop Gram and hepatorenal damage.Long Term Contact low concentration formaldehyde can have slight eye and upper respiratory tract irritation, skin It is dried, chaps.
In indoor environment, formaldehyde mostlys come from furniture and fabric, woodwork filler, building source, cleaning Agent, cosmetics and personal belongings etc., the most mainly artificial board.According to GB/T18883-2002 " room Interior air quality standard ", the content of formaldehyde in air answers≤0.10mg/m3, and first in current room air Aldehyde, the most all beyond national standard, brings the most serious threat therefore to the health of people.
Kieselguhr is a kind of biogenic silicastone, is the Diatomeae of growth in ocean or lake Remains are at subaqueous deposit, a kind of nonmetallic mineral gradually formed through natural environment effect.Kieselguhr master The states such as China to be distributed in, the U.S., Denmark, France, Romania.It is a kind of biogenic siliceous Sedimentary rock, it is mainly made up of the remains of diatom in ancient times.China's kieselguhr reserves 3.2 hundred million tons, distant view Reserves reach more than 20 hundred million tons, are concentrated mainly on East China and the Northeast, and larger, reserves are more Have Jilin (54.8%), Zhejiang, Yunnan, Shandong, Sichuan etc. save.
Diatomaceous density 1.9-2.3g/cm3, bulk density 0.34-0.65g/cm3, specific surface area 40-65m/g, Pore volume 0.45-0.98m, water absorption rate is 2-4 times of own vol, and fusing point 1650C-1750 DEG C, at electricity It is observed that the structure of special porous under sub-microscope.Kieselguhr has certain chemism, simultaneously Architectural feature because of its uniqueness so that kieselguhr have exquisiteness, loose, light weight, porous, water absorption and The physical property that permeability is strong.
Have much based on diatomaceous material, but still suffer from a lot of problem demanding prompt solution.From product See on functional effect, owing to excessively emphasizing and relying on the performance that kieselguhr is single, though using kieselguhr in a large number, But there is no adsorption-decomposition function formaldehyde, noxious odor effect inconspicuous.Also a large amount of compounding Kaolin of having, The mineral powder of mica group, just contains substantial amounts of kaolinite and micaceous clay in the most diatomaceous associated minerals Ore deposit, also adds significantly manufacturing cost while causing waste of material.
The above product also exists the shortcoming that can not be ignored.Such as kieselguhr itself does not possess gelling, If in order to improve its caking property and intensity, use the reinforcing materials such as such as cement to be combined, cause silicon Diatomaceous earth not only cannot recycle, and limits diatomaceous adsorption function, and the most direct effect is exactly Absorption property declines.Some use bonded adhesive, plug diatomaceous small pore, cause point Solve formaldehyde ability to decline.
In view of the importance of formaldehyde and hazardness and kieselguhr are as not enough the asking of function of filtering material Topic, it is necessary to the material that can fully excavate diatomaceous strainability especially suction strainer formaldehyde function is provided And method.
Summary of the invention
Above-mentioned one or more present in process are used to ask to solve kieselguhr as filtering material Topic, the invention provides a kind of for preparation method based on diatomaceous granular filter material, by the party What method prepared inhales at air filtration especially formaldehyde based on diatomaceous granular filter material and this material Application in filter.
The present invention provides a kind of based on diatomaceous granular filter material for preparation in first aspect Method, it is characterised in that described method comprises the steps:
(1) diatomite powder is obtained;
(2) by described diatomite powder and monoacidic base aqueous solution steaming and decocting, it is thus achieved that kieselguhr cooking liquor;
(3) described kieselguhr cooking liquor is filtered, it is thus achieved that kieselguhr steaming and decocting filtrate;
(4) add glycerol to described kieselguhr steaming and decocting filtrate and stir, obtaining the first mixture;
(5) in described first mixture, add polyvinylpyrrolidone and stir, obtaining the second mixing Thing;
(6) in described second mixture, add ethanol and stir, obtaining the 3rd mixture;
(7) by the pH regulator of described 3rd mixture to pH 5 to 6, then stand to gelling in room temperature, Obtain the first kieselguhr gel;
(8) by described first kieselguhr soak 12 hours to 18 hours in ethanol, the second silicon is obtained Diatomaceous earth gel;
(9) described second kieselguhr gel is carried out supercritical drying, obtain described based on diatomaceous powdery Filtering material.
The present invention second aspect provide by the method described in first aspect present invention prepare based on silicon The granular filter material of diatomaceous earth.
The present invention the third aspect provide described in first or second aspect of the present invention based on diatomaceous Granular filter material application in air filtration, the especially application in formaldehyde suction strainer.
What the inventive method prepared has lightweight, highly effective air based on diatomaceous granular filter material Filter the ability of especially formaldehyde suction strainer, may be used for indoor air filtration, such as, can be made into filter element It is put in the air channel of air conditioner.
Detailed description of the invention
Hereafter by way of example the present invention will be carried out further by providing some specific embodiments Description.But the technical scheme that the application is claimed is not limited to these specific embodiments.
The present invention provides a kind of based on diatomaceous granular filter material for preparation in first aspect Method, it is characterised in that described method comprises the steps:
(1) diatomite powder is obtained;
(2) by described diatomite powder and monoacidic base aqueous solution steaming and decocting such as 4 to 6 hours, for example, 4, 5 or 6 hours, it is thus achieved that kieselguhr cooking liquor;If digestion time is long, one is to cause the most too much, Two is to cause Secondary cases to be condensed;If digestion time is too short, leach deficiency;
(3) described kieselguhr cooking liquor is filtered, it is thus achieved that kieselguhr steaming and decocting filtrate;
(4) add glycerol to described kieselguhr steaming and decocting filtrate and stir, obtaining the first mixture;
(5) in described first mixture, add polyvinylpyrrolidone and stir, obtaining the second mixing Thing;
(6) in described second mixture, add ethanol and stir, obtaining the 3rd mixture;
(7) by the pH regulator of described 3rd mixture to pH 5 to 6, then stand to gelling in room temperature, Obtain the first kieselguhr gel;The inventors discovered that, if pH is too low or too high, all can occur coagulating Poly-sedimentation phenomenon;
(8) by described first kieselguhr soak 12 hours to 18 hours in ethanol, the second silicon is obtained Diatomaceous earth gel;If soak time is too short, the second aging deficiency of kieselguhr gel obtained, if soaked Overlong time, extend prepare long while also result in the contraction of the second kieselguhr gel;
(9) described second kieselguhr gel is carried out supercritical drying, obtain described based on diatomaceous powdery Filtering material.
In some embodiments, described diatomite powder preferably has the grain of 20 microns to 100 microns Footpath, for example, 20,30,40,50,60,70,80,90 or 100 microns, further preferred It is that there is the particle diameter of 50 microns to 80 microns.Particle diameter is too low, can cause the original microcellular structure of kieselguhr Destruction;Particle diameter is too high, significantly reduces leaching velocity and efficiency.
In some embodiments, in terms of the weight of described diatomite powder, the consumption of described alkali liquor is preferred It is 50 grams/mol to 150 grams/mol, for example, 50,60,70,80,90,100,120 or 150 Gram/mol;It is further preferred that the consumption of described alkali liquor is preferably 80 grams/mol to 120 grams/mol. Some preferred embodiment in, described monoacidic base aqueous solution is sodium hydroxide or potassium hydroxide solution, Particularly preferably sodium hydroxide solution.
In some embodiments, the boiling temperature in step (2) is 80 DEG C to 90 DEG C, for example, 80 DEG C, 85 DEG C or 90 DEG C.If boiling temperature is too high, filtrate color can be caused the deepest.
In some embodiments, with the stereometer of described kieselguhr steaming and decocting filtrate, the consumption of described glycerol It is 5 volume % to 10 volume %, for example, 5,6,7,8,9 or 10 volume %.If glycerol Consumption is too low, causes the last dusty material microcellular structure skewness prepared;If the consumption of glycerol Too high, then may delay gelation rate, even cannot form gel.
In some embodiments, with the stereometer of described kieselguhr steaming and decocting filtrate, described polyvinyl pyrrole The quality percent by volume of alkanone (PVP) is 6% to 10%, for example, 5,6,7,8,9 or 10%. If the amount of PVP is very few, gelation rate is the slowest.It may further be preferable that the molecular weight of PVP is preferred It is 4000 to 6000, for example, 4000,4500,5000,5500 or 6000.The present inventor is in advance It was found that, the molecular weight of PVP is too low, the speed mistake of final gained granular filter material suction strainer formaldehyde And be unfavorable for the regeneration to granular filter material slowly,;If the molecular weight of PVP is too high, it is unfavorable for The stable capture of formaldehyde, is easily caused the effusion of captured formaldehyde.
In some embodiments, with the stereometer of described kieselguhr steaming and decocting filtrate, the consumption of described ethanol It is 25 volume % to 30 volume %, for example, 25,26,27,28,29 or 30 volume %.
Can be notable it is a discovery of the invention that add glycerol, PVP and ethanol successively with consumption in the order described above Improve the ability of the last granular filter material prepared capture formaldehyde, thus it is speculated that be possibly due to glycerol, PVP The microcellular structure working in coordination with change gained granular filter material with ethanol (is likely to reduce, because formaldehyde divides Son is generally less than little an order of magnitude of micro-pore diameter of gained granular filter material) and distributing homogeneity.Order If people is it was unexpected that exchange the order of addition of glycerol and ethanol, find that gained granular filter material is caught Obtain the ability of formaldehyde.
The present invention second aspect provide by the method described in first aspect present invention prepare based on silicon The granular filter material of diatomaceous earth.It is of course also possible to the described further pelletize of powder filter material is used.
The present invention the third aspect provide described in first or second aspect of the present invention based on diatomaceous Granular filter material application in air filtration, the especially application in formaldehyde suction strainer.It is to be understood that It is that described powder filter material can be used for fluid other impurity of such as water such as antibacterial, virus, powder The suction strainer of dirt etc..
It is further noted that, if not otherwise specified, any scope described in the present invention includes end value And any numerical value between end value and and being constituted with any number between end value or end value Anyon scope.
Below in conjunction with embodiment, the invention will be further described.These embodiments are excellent with regard to the present invention Selecting embodiment to be illustrated, protection scope of the present invention is not read as pertaining only to these and implements Example.
Embodiment
Hereafter by the form of embodiment, the present invention will be further detailed.
Embodiment 1
Weigh and pulverized, by the one-level kieselguhr produced from Linjiang, the diatomite powder 100g obtained, add Enter the sodium hydrate aqueous solution of 0.5 mole/L, and 85 DEG C of steaming and decoctings 7.5 hours, it is thus achieved that kieselguhr steaming and decocting Liquid.Described kieselguhr cooking liquor is filtered, it is thus achieved that kieselguhr steaming and decocting filtrate.Filter to described kieselguhr steaming and decocting Liquid adds glycerol and stirs, and then adds polyvinylpyrrolidone and stirs, then adding ethanol And stir.By pH regulator to pH 6, and stand 12 hours in room temperature, obtain the first kieselguhr Gel.By described first kieselguhr soak 12 hours in ethanol, period often soaked 4 hours more Change an ethanol, obtain the second kieselguhr gel.Then, described second kieselguhr gel is carried out super facing Boundary is dried, and obtains described based on diatomaceous granular filter material.
Obtained granular filter material is filled into a diameter of 40cm, the tubulose of a length of 20cm holds Also jolt ramming in device, two terminal inner lining layer of non-woven fabric of granular filter material, outer lining polypropylene net uses opening again A diameter of 38cm, external diameter are that the end cap of 40cm is threaded connection fixing, thus form round pie Filter element, then filter element is placed on content of formaldehyde is 0.200mg/m330m3Cabin in, then Use aerator (M5-36 type, purchased from Jiangsu Heng Yuan aerator company limited) with the most high-grade air blast 20 minutes. The content of formaldehyde of the cabin indoor gas after using test air blast to process immediately after, calculates according to equation below Air blast process formaldehyde suction strainer rate and by result arrange in table 1 below: formaldehyde suction strainer rate=(0.200-process after Concentration)/0.200x 100%.
Embodiment 2 to 20
In addition to content shown in table 1, prepare granular filter material in the same manner as example 1 also And measure formaldehyde suction strainer rate in an identical manner.
Embodiment 21
Except first to add ethanol, then to add PVP that molecular weight is 5000, add the suitable of glycerol again Sequence is added outside ethanol, PVP and glycerol, prepares granular filter material also in the way of identical with embodiment And measure formaldehyde suction strainer rate in an identical manner.
Embodiment 22
Use the silicon alkoxide of 100g and ethanol, deionized water, ammonia in parts by weight: 1: 10: 10: 0.01 (mol ratio) proportioning is configured to colloidal sol, adds glycerol to described kieselguhr steaming and decocting filtrate and stirs, Then add polyvinylpyrrolidone and stir, then add ethanol and stir.By pH regulator To pH 6, and stand 12 hours in room temperature, obtain the first kieselguhr gel.By described first kieselguhr Soak 12 hours in ethanol, period often soak 4 hours change an ethanol, obtain the second silicon Diatomaceous earth gel.Then, described second kieselguhr gel is carried out supercritical drying, obtains based on kieselguhr Granular filter material, and in an identical manner measure formaldehyde suction strainer rate, result is listed in the table below in 1.
Embodiment 23
The circle forming size same as in Example 1 is directly loaded with the diatomite powder that particle diameter is 60 microns Pie filter element, and measure formaldehyde suction strainer rate in an identical manner, result is listed in the table below in 1.
Table 1 raw material and reagent dosage, preparation process parameter and the formaldehyde of obtained granular filter material Suction strainer rate.

Claims (10)

1. one kind is used for preparation method based on diatomaceous granular filter material, it is characterised in that institute The method of stating comprises the steps:
(1) diatomite powder is obtained;
(2) by described diatomite powder and monoacidic base aqueous solution steaming and decocting 7.5 hours, it is thus achieved that kieselguhr cooking liquor;
(3) described kieselguhr cooking liquor is filtered, it is thus achieved that kieselguhr steaming and decocting filtrate;
(4) add glycerol to described kieselguhr steaming and decocting filtrate and stir, obtaining the first mixture;
(5) in described first mixture, add polyvinylpyrrolidone and stir, obtaining the second mixing Thing;
(6) in described second mixture, add ethanol and stir, obtaining the 3rd mixture;
(7) by the pH regulator of described 3rd mixture to pH 5 to 6, then stand to gelling in room temperature, Obtain the first kieselguhr gel;
(8) by described first kieselguhr soak 12 hours to 18 hours in ethanol, the second silicon is obtained Diatomaceous earth gel;
(9) described second kieselguhr gel is carried out supercritical drying, obtain described based on diatomaceous powdery Filtering material.
Method the most according to claim 1, it is characterised in that described diatomite powder has 20 The particle diameter of micron to 100 microns.
Method the most according to claim 1 and 2, it is characterised in that the steaming and decocting temperature in step (2) Degree is 80 DEG C to 90 DEG C.
Method the most according to claim 1 and 2, it is characterised in that with described kieselguhr steaming and decocting The stereometer of filtrate, the consumption of described glycerol is 5 volume % to 10 volume %.
Method the most according to claim 1 and 2, it is characterised in that with described kieselguhr steaming and decocting The stereometer of filtrate, the quality percent by volume of described polyvinylpyrrolidone is that 6 mass % are to 10 matter Amount %.
Method the most according to claim 1 and 2, it is characterised in that with described kieselguhr steaming and decocting The stereometer of filtrate, the consumption of described ethanol is 25 volume % to 30 volume %.
Method the most according to claim 1 and 2, it is characterised in that described monoacidic base aqueous solution For sodium hydrate aqueous solution or potassium hydroxide aqueous solution.
8. by the method described in claim 1 or 2 prepare based on diatomaceous granular filter material.
9. described in claim 8 based on diatomaceous granular filter material in air filtration should With.
10. described in claim 8 based on diatomaceous granular filter material in formaldehyde suction strainer should With.
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CN106111091B (en) * 2016-07-26 2018-12-18 东莞市晶谷新材料技术有限公司 A kind of diatom soil matrix is except formaldehyde composite material for air cleaning and preparation method thereof
CN107970887A (en) * 2017-11-22 2018-05-01 大连智讯科技有限公司 A kind of preparation method of konilite

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CN1864851A (en) * 2006-04-13 2006-11-22 浙江三鼎科技有限公司 Method for preparing modified composite absorption agent of diatomite
CN102343253B (en) * 2011-08-12 2012-08-15 江苏赢海美联新材料科技有限公司 Filtering sorbent material, its preparation method and its application
US8999361B2 (en) * 2011-10-25 2015-04-07 Jack L. Mathis Silane modified diatomaceous earth mechanical insecticide
CN102641720A (en) * 2012-04-01 2012-08-22 华南师范大学 Preparation method for modified kieselguhr composite adsorbing material
CN103894015B (en) * 2014-04-15 2016-01-27 刁广祥 Composite diatomite filtering material
CN104437350A (en) * 2015-01-06 2015-03-25 华北水利水电大学 Kieselguhr-based particle adsorbent and preparation and modification method thereof

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