CN116116383A - Black talcum-based composite air purifying agent and preparation method thereof - Google Patents

Black talcum-based composite air purifying agent and preparation method thereof Download PDF

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CN116116383A
CN116116383A CN202211445597.1A CN202211445597A CN116116383A CN 116116383 A CN116116383 A CN 116116383A CN 202211445597 A CN202211445597 A CN 202211445597A CN 116116383 A CN116116383 A CN 116116383A
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black
based composite
composite air
air purifying
purifying agent
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张国亮
陈宇
王玲
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Zhejiang University of Technology ZJUT
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Abstract

The invention discloses a black talcum-based composite air purifying agent and a preparation method thereof, belonging to the field of comprehensive utilization of nonmetallic minerals. The method comprises the following steps: and etching the black talcum after ball milling to increase the specific surface area and the porosity of the black talcum, so that the surface of the black talcum is rich in active functional groups, then grafting, grafting active groups to increase the adsorption quantity of formaldehyde, and finally compounding and granulating with mercerized zeolite to obtain the small microsphere. The advantages of the graphene-like layer, the lamellar structure and the like of the black talcum are effectively utilized. The preparation process is simple, the raw materials are cheap and easy to obtain, the adsorption effect is good, the production scale is easy to control, the environment is protected, and no secondary pollution is generated. The invention provides a new direction for the production field of the adsorbent, reduces the cost of the existing adsorbent, and provides an effective, economical and practical way for improving the comprehensive utilization of the black talc ore.

Description

Black talcum-based composite air purifying agent and preparation method thereof
Technical Field
The invention belongs to the field of comprehensive utilization of nonmetallic minerals, and particularly relates to a black talc-based composite air purifying agent and a preparation method thereof.
Background
The most main indoor pollution source is formaldehyde, and the national sanitation standard prescribes that the indoor formaldehyde concentration is not more than 0.08mg/m 3 Especially in the room after the fitment, formaldehyde concentration seriously exceeds standard, brings very big influence to human health, and the commercial formaldehyde adsorbent of present stage is the active carbon package almost, but active carbon package adsorption capacity is less, is difficult to regenerate for remove formaldehyde thoroughly, still has the problem of with high costs.
The black smooth stone ore has black color, purer chemical composition, fine particles, flaky structure, higher specific surface area, no asbestos harmful minerals, huge reserve, lower exploitation cost and low price, and is widely used in industrial products such as ceramics, papermaking, fillers and the like. The vast majority of the black talc products are low-end products such as fillers, and there is still a great development space in other high-end technology fields. The properties of the black talc can be reasonably utilized for modification, and the performance of the black talc in other aspects is improved. The technology not only accords with the novel industrial road and sustainable development strategy in China, but also widens the application field of the black talc and increases the economic benefit brought by the black talc industry.
Disclosure of Invention
Aiming at the problems of higher development cost and lower adsorption capacity of the existing activated carbon formaldehyde adsorbent, the invention provides a preparation method of a black talc-based composite air purifying agent. The air purifying agent is synthesized through steps of etching, grafting, compounding and the like, has simple operation process, good adsorption effect on formaldehyde and other air polar pollutants, and has high recovery efficiency.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention provides a black talc-based composite air purifying agent, which is prepared by the following steps:
(1) Etching of black talc: immersing black talc powder with the average particle size of 200-500 nm (preferably 300-400 nm) into an aqueous solution of alkaline substances with the total concentration of 1-4 mol/L (preferably 2 mol/L), heating and stirring at 60-90 ℃ for 6-10 hours (preferably 70 ℃ for 7 hours), and carrying out post-treatment A on the obtained reaction solution A to obtain etched black talc powder; the alkaline substance in the aqueous solution of the alkaline substance is one or more than two of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate and ammonium hydroxide (ammonia water).
The etching aims to etch part of silicon between the lamellar layers of the black talc, so that the pore channel structure of the black talc is more abundant, and the surface of the black talc is rich in active functional groups.
(2) Adding the etched black talcum powder obtained in the step (1) into an organic solvent, adding a grafting agent, carrying out grafting reaction for 3-8 hours (preferably 5 hours) at 50-90 ℃ (preferably 70 ℃), and carrying out post-treatment on the obtained reaction liquid B to obtain grafted black talcum powder; the grafting agent is one or more than two of N-beta- (aminoethyl) -gamma-aminopropyl trimethoxysilane (KH 792), gamma-aminopropyl triethoxysilane (KH 550), gamma-glycidoxypropyl trimethoxysilane (KH 560) and gamma-mercaptopropyl trimethoxysilane (KH 590) (preferably N-beta- (aminoethyl) -gamma-aminopropyl trimethoxysilane); the mass ratio of the grafting agent to the etched black talcum powder is 1:1-3 (preferably 1:1);
the grafting aims to graft hydroxyl rich on the surface of the black talcum, and the grafting is carried out with active groups so as to increase the adsorption quantity of formaldehyde.
(3) The grafted black talcum powder, mercerized zeolite powder with the average particle diameter of 200-500 nm (preferably 300-400 nm) and the binder are mixed and granulated to obtain the black talcum-based composite air purifying agent; the mass ratio of the grafted black talcum powder to the mordenite to the binder is 1:0.5 to 3:0.2 to 0.5 (preferably 1:1:0.33).
Further, the volume of the aqueous solution of the alkaline substance in the step (1) is 1 to 5mL/g (2.5 mL/g) based on the mass of the black talc powder.
Further, the post-treatment in step (1) is: the reaction solution was cooled to room temperature, centrifuged (in one embodiment of the invention, 5000rpm/min for 5 min), and the obtained precipitate was centrifugally washed with deionized water to neutrality, dried, and sieved (200 mesh) to obtain etched black talc powder.
Further, the organic solvent in the step (2) is one or more of toluene, ethanol, methanol, and acetone (preferably, one or more of methanol and toluene, and most preferably, toluene).
Preferably, the volume of the organic solvent in the step (2) is 1 to 5ml/g (3 ml/g) based on the mass of the etched black talc powder.
Further, the post-treatment B in step (2) is: and (3) cooling the reaction liquid B, centrifuging, re-suspending and washing the obtained precipitate with absolute ethyl alcohol for three times, drying the obtained lower layer solid (60 ℃), grinding and sieving (200 meshes) to obtain the grafted black talcum powder.
Further, the binder in the step (3) is one or a mixture of more than two of polyvinyl alcohol (PVA), sodium carbonate and ethyl orthosilicate (preferably polyvinyl alcohol).
In one embodiment of the invention, the speed of rotation of the granulation in step (3) is 32r/min, resulting in spherical particles with a diameter of 2-3 mm. The rotating speed can be set according to the requirement in actual production.
The invention provides a black talc powder having an average particle diameter of 200 to 500nm (preferably 300 to 400 nm) in the step (1), which is prepared by the following method: crushing, grinding and sieving black talc (200 meshes) in Guangfeng region of Shangshi, jiangxi province to obtain black talc powder, adding ethanol and deionized water into the black talc powder, ball milling in a ball mill by a wet method, taking out a sample, re-suspending and washing with deionized water, taking out the solid at the lower layer in a centrifuge tube, drying, grinding and sieving (200 meshes) to obtain superfine black talc powder with the average particle diameter of 200-500 nm; the volume ratio of the ethanol to the deionized water is 0.5-2:1 (preferably 1:1); the total volume of ethanol and deionized water is based on complete immersion of the black talc powder. Preferably, the volume of the ethanol is 0.6-1.6mL/g based on the mass of the black talc powder. The rotational speed of the wet ball milling is 700-800 r/min, and the time is 8-10 h. The drying temperature is 60-120 ℃ (preferably 80-100 ℃) and the drying time is 12-15 hours.
The invention provides a mercerized zeolite powder with the average grain diameter of 200-500 nm (preferably 300-400 nm) in the step (3), which is prepared by the following method: crushing mordenite (Jiangsu Jinyun), grinding, sieving (200 meshes) to obtain mordenite powder, adding ethanol and deionized water into the mordenite powder, performing wet ball milling in a ball mill, taking out a sample, performing deionized water resuspension washing, taking out the lower solid in a centrifuge tube, drying, grinding and sieving (200 meshes) to obtain superfine mordenite powder, wherein the average particle size of the superfine mordenite powder is 200-500 nm; the volume ratio of the ethanol to the deionized water is 0.5-2:1 (preferably 1:1); the total volume of ethanol and deionized water is based on complete immersion of the black talc powder. Preferably the volume of ethanol is from 0.6 to 1.6mL/g based on the mass of the mordenite powder. The rotational speed of the wet ball milling is 700-800 r/min, and the time is 8-10 h. The drying temperature is 60-120 ℃ (preferably 80-100 ℃) and the drying time is 12-15 hours.
The invention also provides application of the black talc-based composite air purifying agent in formaldehyde adsorption.
Compared with the existing materials, the invention has the beneficial effects that: the black talc is ball-milled, the specific surface area of the black talc is effectively increased, the black talc is etched, the surface is rich in active groups, the specific surface area is further increased, pore channels are enriched, the grafting activation is carried out, the structure of a graphene-like layer is reserved, the active groups are rich on the surface, and finally the mercerized zeolite with high adsorption capacity is compounded, so that the adsorption capacity of formaldehyde is greatly increased. The preparation process is simple, the raw materials are cheap and easy to obtain, the production scale is easy to control, the environment is protected, and no secondary pollution is generated. The invention provides a new direction for the field of black talcum adsorbents, and simultaneously provides an effective, economical and practical way for improving the comprehensive utilization of the black talcum ores.
Drawings
FIG. 1 FT-IR chart of the black talc before and after grafting in example 1.
Detailed Description
The present invention will be further described with reference to specific examples, but the present invention is not limited to the following examples, and various modifications are intended to be included within the technical scope of the present invention without departing from the spirit and scope of the present invention.
The formaldehyde testing method comprises the following steps: placing formaldehyde detector (kanfar JQ151 type) in a sealed glass container with dimensions of 30cm×30cm, introducing formaldehyde into the sealed chamber, and ensuring formaldehyde concentration at 0.5mg/m 3 Then 50g of adsorbent particles are put into the mixture for adsorption, the reading of a formaldehyde detector is observed after 5 hours, and the formaldehyde adsorption rate is calculated. A blank is placed.
Example 1
(1) The following conditions for preparing the black talc powder were: taking black talcum from Guangfeng of Jiangxi, crushing, grinding, sieving (200 meshes) to obtain black talcum powder, adding 80ml of ethanol and 80ml of deionized water into 100g of black talcum powder, placing into a ball mill, grinding by a wet method at a rotating speed of 800r/min for 10 hours, taking out a sample, re-suspending and washing by the deionized water, centrifuging for three times, taking out the solid at the lower layer in a centrifuge tube, drying at 80 ℃ for 12 hours, grinding and sieving (200 meshes) to obtain superfine black talcum powder, wherein the average particle size of the superfine black talcum powder is 300nm.
(2) Etching of black talc: taking 80g of the superfine black talc powder in the step (1), heating and stirring in a water bath of 70 ℃ in 200ml of 2mol/L NaOH solution for 7h, cooling to room temperature, centrifuging at 5000rpm/min for 5min, re-suspending and washing with deionized water until the supernatant is neutral, drying, grinding and sieving (200 meshes) to obtain etched black talc powder;
(3) Preparation of grafted black talc: placing 80g of etched black talc in the step (2) in 240ml of toluene, adding 80g of KH792, placing in a reaction kettle, heating at 70 ℃ for 5 hours, cooling, centrifuging to remove the lower layer solid, adding absolute ethyl alcohol, carrying out resuspension washing, centrifuging, repeating for three times, removing the lower layer solid, drying at 60 ℃, taking out, grinding and sieving (200 meshes) to obtain grafted black talc.
(4) Preparation of mordenite: selecting a Jinyun zeolite ore produced in Jiangsu, yun, crushing, and ball-milling in the mode of the step (1), wherein the average grain size is 300nm.
(5) Black talc based composite air cleaner: 30g of grafted black talcum powder, 30g of mordenite and 10g of PVA are taken and granulated in a disc granulator at the speed of 32r/min, so as to obtain spherical particles with the diameter of 2-3 mm. Wherein the mercerized Jinyun zeolite is formed by crushing Jinyun zeolite ore.
(6) The formaldehyde removal rate of the obtained product is 97.8%.
Example 2
The other operations were the same as in example 1, except that the grafting agent in step (3) was different in kind and the other conditions were the same. The grafting agent species used are listed in the table below.
Name of the name Formaldehyde adsorption rate (%)
80g KH550 96.0
80g KH560 91.2
80g KH590 93.5
80g of triethanolamine 86.2
80g of p-aminobenzenesulfonic acid 89.5
80g of hexamethylenetetramine 81.3
Example 3
The other operations were the same as in example 1, except that the binder type in step (5) was different, and the other conditions were the same. The grafting agent species used are listed in the table below.
Figure BDA0003949524050000071
Figure BDA0003949524050000081
Example 4
The other operations were identical to example 1, except that the mass ratio of black talc to mordenite in step (5) was different, all other conditions being identical. The grafting agent species used are listed in the table below.
Figure BDA0003949524050000082
Example 5
The other operations were the same as in example 1, except that the organic solvent in step (3) was different in kind and the other conditions were the same. The grafting agent species used are listed in the table below.
Name of the name Formaldehyde adsorption rate (%)
240ml of ethanol 87.1
240ml of methanol 90.2
240ml of acetone 86.4
Comparative example 1
(1) The following conditions for preparing the black talc powder were: taking black talcum from Guangfeng of Jiangxi, crushing, grinding, sieving (200 meshes) to obtain black talcum powder, adding 80ml of ethanol and 80ml of deionized water into 100g of black talcum powder, placing into a ball mill, grinding by a wet method at a rotating speed of 800r/min for 10 hours, taking out a sample, re-suspending and washing by the deionized water, centrifuging for three times, taking out the solid at the lower layer in a centrifuge tube, drying at 80 ℃ for 12 hours, grinding and sieving (200 meshes) to obtain superfine black talcum powder, wherein the average particle size of the superfine black talcum powder is 300nm.
(2) Etching of black talc: taking 80g of the superfine black talc powder in the step (1), heating and stirring in a water bath of 70 ℃ in 200ml of 2mol/L NaOH solution for 7h, cooling to room temperature, centrifuging at 5000rpm/min for 5min, re-suspending and washing with deionized water until the supernatant is neutral, drying, grinding and sieving (200 meshes) to obtain etched black talc powder;
(3) Preparation of grafted black talc: and (3) placing 80g of etched black talc in the step (2) in 240ml of toluene, adding 80g of KH792, placing in a reaction kettle, heating at 70 ℃ for 5 hours, cooling, centrifuging to remove the lower layer solid, adding absolute ethyl alcohol, re-suspending, washing, centrifuging, repeating for three times, taking the lower layer solid, drying at 60 ℃, taking out, grinding and sieving (200 meshes) to obtain grafted black talc.
(4) Black talc based air cleaner: 60g of grafted black talc and 10g of PVA are granulated in a granulator to obtain spherical particles with diameters of 2-3 mm.
(5) The formaldehyde removal rate of the obtained product is 62%.
Comparative example 2
(1) Mordenite zeolite: 60g of mercerized Jinyun zeolite and 10g of PVA are taken out in a granulator for granulation, and spherical particles with the diameter of 2-3 mm are obtained.
(2) The formaldehyde removal rate of the obtained product is 40%.
Comparative example 3
(1) The following conditions for preparing the black talc powder were: taking black talcum from Guangfeng of Jiangxi, crushing, grinding, sieving (200 meshes) to obtain black talcum powder, adding 80ml of ethanol and 80ml of deionized water into 100g of black talcum powder, placing into a ball mill, grinding by a wet method at a rotating speed of 800r/min for 10 hours, taking out a sample, re-suspending and washing by the deionized water, centrifuging for three times, taking out the solid at the lower layer in a centrifuge tube, drying at 80 ℃ for 12 hours, grinding and sieving (200 meshes) to obtain superfine black talcum powder, wherein the average particle size of the superfine black talcum powder is 300nm.
(2) Etching of black talc: taking 80g of the superfine black talc powder in the step (1), heating and stirring in a water bath of 70 ℃ in 200ml of 2mol/L NaOH solution for 7h, cooling to room temperature, centrifuging at 5000rpm/min for 5min, re-suspending and washing with deionized water until the supernatant is neutral, drying, grinding and sieving (200 meshes) to obtain etched black talc powder;
(3) Preparation of mordenite: selecting and crushing a Jinyun zeolite ore produced in Jiangsu, and ball-milling in the mode of the step (1), wherein the particle size of the Jinyun zeolite ore is the same as that of the black talc.
(4) Black talc based composite air cleaner: 30g of black talcum powder, 30g of mordenite zeolite and 10g of PVA are taken and granulated in a disc granulator at the speed of 32r/min, so as to obtain spherical particles with the diameter of 2-3 mm. Wherein the mercerized Jinyun zeolite is formed by crushing Jinyun zeolite ore.
(5) The formaldehyde removal rate of the obtained product is 73.7%.

Claims (10)

1. The black talc-based composite air purifying agent is characterized by being prepared by the following steps:
(1) Etching of black talc: immersing black talcum powder with the average grain diameter of 200-500 nm into an aqueous solution of alkaline substances with the total concentration of 1-4 mol/L, heating and stirring at 60-90 ℃ for 6-10 hours, and carrying out post-treatment A on the obtained reaction solution A to obtain etched black talcum powder; the alkaline substance in the aqueous solution of the alkaline substance is one or more than two of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate and ammonium hydroxide.
(2) Adding the etched black talcum powder obtained in the step (1) into an organic solvent, adding a grafting agent, and carrying out grafting reaction for 3-8 hours at 50-90 ℃, wherein the obtained reaction liquid B is subjected to post-treatment B to obtain grafted black talcum powder; the grafting agent is one or more than two of N-beta- (aminoethyl) -gamma-aminopropyl trimethoxysilane, gamma-aminopropyl triethoxysilane, gamma-glycidol ether oxypropyl trimethoxysilane and gamma-mercaptopropyl trimethoxysilane; the mass ratio of the grafting agent to the etched black talcum powder is 1:1-3;
(3) The grafted black talcum powder, mercerized zeolite powder with the average grain diameter of 200-500 nm and the binder are mixed and granulated to obtain the black talcum-based composite air purifying agent; the mass ratio of the grafted black talcum powder to the mordenite to the binder is 1:0.5 to 3:0.2 to 0.5.
2. The black talc-based composite air purifying agent according to claim 1, wherein: the volume of the aqueous solution of the alkaline substance in the step (1) is 1 to 5mL/g based on the mass of the black talc powder.
3. The black talc-based composite air purifying agent according to claim 1, wherein: the post-treatment in the step (1) is as follows: and cooling the reaction liquid to room temperature, centrifuging, centrifugally washing the obtained precipitate with deionized water to neutrality, drying, and sieving to obtain etched black talcum powder.
4. The black talc-based composite air purifying agent according to claim 1, wherein: the grafting agent in the step (2) is N-beta- (aminoethyl) -gamma-aminopropyl trimethoxysilane.
5. The black talc-based composite air purifying agent according to claim 1, wherein: the organic solvent in the step (2) is one or a mixture of more than two of toluene, ethanol, methanol and acetone.
6. The black talc-based composite air purifying agent according to claim 1, wherein: the organic solvent in the step (2) is one or a mixture of more than two of methanol and toluene.
7. The black talc-based composite air purifying agent according to claim 1, wherein: the volume of the organic solvent in the step (2) is 1-5 ml/g based on the mass of the etched black talcum powder.
8. The black talc-based composite air purifying agent according to claim 1, wherein: the post-treatment B in the step (2) is as follows: and (3) cooling the reaction liquid B, centrifuging, re-suspending and washing the obtained precipitate with absolute ethyl alcohol for three times, drying the obtained lower layer solid, grinding and sieving to obtain the grafted black talcum powder.
9. The black talc-based composite air purifying agent according to claim 1, wherein: the binder in the step (3) is one or a mixture of more than two of polyvinyl alcohol, sodium carbonate and tetraethoxysilane.
10. Use of the black talc based composite air cleaner according to claim 1 for adsorbing formaldehyde.
CN202211445597.1A 2022-11-18 2022-11-18 Black talcum-based composite air purifying agent and preparation method thereof Pending CN116116383A (en)

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CN1554447A (en) * 2003-12-26 2004-12-15 杜建中 Super fine active compound adsorptive indoor air purifying agent
CN101254924A (en) * 2008-04-09 2008-09-03 中国科学院化学研究所 Silicane coupling agent surface grafted modified clay as well as preparation method and use thereof
JP2009136832A (en) * 2007-12-10 2009-06-25 National Institute Of Advanced Industrial & Technology Natural mineral membrane
CN103084144A (en) * 2013-02-06 2013-05-08 中国科学院广州地球化学研究所 Diatomite-based porous composite material for adsorbing volatile organic pollutants and preparation method thereof
CN113731364A (en) * 2021-09-17 2021-12-03 苏州中材非金属矿工业设计研究院有限公司 Black talc adsorbent and preparation method and application thereof
CN114989494A (en) * 2022-06-30 2022-09-02 中国地质大学（武汉） Modified black talc antibacterial material and dry preparation process and application thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1554447A (en) * 2003-12-26 2004-12-15 杜建中 Super fine active compound adsorptive indoor air purifying agent
JP2009136832A (en) * 2007-12-10 2009-06-25 National Institute Of Advanced Industrial & Technology Natural mineral membrane
CN101254924A (en) * 2008-04-09 2008-09-03 中国科学院化学研究所 Silicane coupling agent surface grafted modified clay as well as preparation method and use thereof
CN103084144A (en) * 2013-02-06 2013-05-08 中国科学院广州地球化学研究所 Diatomite-based porous composite material for adsorbing volatile organic pollutants and preparation method thereof
CN113731364A (en) * 2021-09-17 2021-12-03 苏州中材非金属矿工业设计研究院有限公司 Black talc adsorbent and preparation method and application thereof
CN114989494A (en) * 2022-06-30 2022-09-02 中国地质大学（武汉） Modified black talc antibacterial material and dry preparation process and application thereof

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