CN108751372B - Silica aerogel doped calcium zeolite water treatment agent and preparation method thereof - Google Patents
Silica aerogel doped calcium zeolite water treatment agent and preparation method thereof Download PDFInfo
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- CN108751372B CN108751372B CN201810747088.1A CN201810747088A CN108751372B CN 108751372 B CN108751372 B CN 108751372B CN 201810747088 A CN201810747088 A CN 201810747088A CN 108751372 B CN108751372 B CN 108751372B
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- calcium zeolite
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- silica aerogel
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- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 59
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 239000010457 zeolite Substances 0.000 title claims abstract description 59
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 48
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 43
- 239000011575 calcium Substances 0.000 title claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000004965 Silica aerogel Substances 0.000 title claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000006185 dispersion Substances 0.000 claims abstract description 22
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 17
- 239000007822 coupling agent Substances 0.000 claims abstract description 14
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 13
- 239000004964 aerogel Substances 0.000 claims abstract description 12
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 12
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims abstract description 11
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 28
- OBFQBDOLCADBTP-UHFFFAOYSA-N aminosilicon Chemical compound [Si]N OBFQBDOLCADBTP-UHFFFAOYSA-N 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 150000001669 calcium Chemical class 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- -1 amino silica aerogel Chemical compound 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 239000012065 filter cake Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims 1
- 239000000292 calcium oxide Substances 0.000 claims 1
- 235000012255 calcium oxide Nutrition 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 6
- 229920002401 polyacrylamide Polymers 0.000 abstract description 5
- 206010024796 Logorrhoea Diseases 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 abstract description 2
- 238000005189 flocculation Methods 0.000 abstract description 2
- 230000016615 flocculation Effects 0.000 abstract description 2
- 238000000034 method Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000010705 motor oil Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a silica aerogel doped calcium zeolite water treatment agent and a preparation method thereof, wherein the water treatment agent is prepared from the following raw materials in parts by weight: 0.1-0.2 part of triethylamine, 5-7 parts of silica aerogel, 100 parts of calcium zeolite, 140 parts of ammonium persulfate, 1-1.3 parts of glycidyl methacrylate, 3-4 parts of aminosilane coupling agent and 40-50 parts of acrylamide. The material adopts the method of coordinative treatment of the silicon dioxide aerogel, the garrulous zeolite powder and the polyacrylamide, has good treatment effect, high stability of a finished product, difficult dispersion, good self-settling effect and convenient recovery, and the silicon dioxide aerogel and the polyacrylamide can be uniformly distributed in the microporous structure of the garrulous zeolite powder, thereby not only improving the flocculation effect, but also being convenient for cleaning, having high recycling rate and being convenient for treatment.
Description
Technical Field
The invention belongs to the field of water treatment agents, and particularly relates to a silica aerogel doped calcium zeolite water treatment agent and a preparation method thereof.
Background
The green water treatment agent is a hotspot of research and development in the field of industrial circulating cooling water at present, and the green water treatment agent which is actively developed and operated to meet the Chinese situation has positive environmental significance and also has important economic value;
the water treatment agent commonly used in the market at present has single functionality, can only treat specific wastewater environment generally, and most of the water treatment agents in the market have elements harmful to the environment, so the invention aims to provide the water treatment agent with good use environmental protection, strong functionality, high use stability and wide application range.
Disclosure of Invention
The invention aims to provide a silica aerogel doped calcium zeolite water treatment agent and a preparation method thereof aiming at the defects and shortcomings of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a silica aerogel doped calcium zeolite water treatment agent is composed of the following raw materials in parts by weight: 0.1-0.2 part of triethylamine, 5-7 parts of silica aerogel, 100 parts of calcium zeolite, 140 parts of ammonium persulfate, 1-1.3 parts of glycidyl methacrylate, 3-4 parts of aminosilane coupling agent and 40-50 parts of acrylamide.
The aminosilane coupling agent is a silane coupling agent kh550.
The preparation method of the silica aerogel doped calcium zeolite water treatment agent comprises the following steps:
(1) adding ammonium persulfate into deionized water with the weight of 20-30 times of that of the ammonium persulfate, and uniformly stirring;
(2) taking the calcium zeolite, sending the calcium zeolite into sodium hydroxide with the concentration of 0.8-1mol/l, soaking for 1-2 hours, discharging, calcining for 1-2 hours at the temperature of 600-700 ℃, cooling, grinding into fine powder, mixing with glycidyl methacrylate, adding into deionized water with the weight of 3-5 times of that of the mixture, and stirring for 2-4 hours at the temperature of 80-90 ℃ to obtain calcium zeolite dispersion liquid;
(3) mixing the silicon dioxide aerogel and the aminosilane coupling agent, adding the mixture into absolute ethyl alcohol with the weight 6-8 times of that of the mixture, raising the temperature to 60-65 ℃, keeping the temperature, stirring for 1-2 hours, and distilling to remove the ethyl alcohol to obtain the amino silicon dioxide aerogel;
(4) adding the amino silica aerogel into the calcium zeolite dispersion liquid, uniformly stirring, raising the temperature to be 170-190 ℃, adding triethylamine, and stirring for 4-7 hours under the condition of heat preservation to obtain a modified calcium zeolite dispersion liquid;
(5) adding acrylamide into the modified calcium zeolite dispersion liquid, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to be 60-75 ℃, adding the ammonium persulfate aqueous solution, keeping the temperature and stirring for 3-5 hours, discharging, performing suction filtration, washing a filter cake, drying for 2-4 hours at the temperature of 50-60 ℃ in vacuum, and cooling to normal temperature to obtain the silica aerogel doped calcium zeolite water treatment agent.
The invention has the advantages that:
the invention takes the calcium zeolite as a raw material, can improve the stability of the microporous structure of the calcium zeolite after being treated in an alkaline solution, then adopts glycidyl methacrylate for treatment, utilizes an epoxy group to bond the epoxy group on the surface of the calcium zeolite, then adopts aminosilane coupling agent to treat silica aerogel, is mixed with epoxy modified calcium zeolite, and is subjected to ring opening at high temperature under the catalytic action of triethylamine, so that the close combination of the calcium zeolite powder and the silica aerogel is realized, the dispersion probability and the dispersion stability of the silica aerogel in the calcium zeolite micropores are increased, then, acrylamide is taken as a monomer to be dispersed in the modified calcium zeolite dispersion liquid, and activated carbon-carbon double bonds in the glycidyl methacrylate can participate in polymerization reaction, thereby realizing the good dispersion compatibility between the polyacrylamide and the silica aerogel doped zeolite powder, thereby improving the mechanical stability of the finished product material;
the material adopts the method of coordinative treatment of the silicon dioxide aerogel, the garrulous zeolite powder and the polyacrylamide, has good treatment effect, high stability of a finished product, difficult dispersion, good self-settling effect and convenient recovery, and the silicon dioxide aerogel and the polyacrylamide can be uniformly distributed in the microporous structure of the garrulous zeolite powder, thereby not only improving the flocculation effect, but also being convenient for cleaning, having high recycling rate and being convenient for treatment.
Detailed Description
Example 1
A silica aerogel doped calcium zeolite water treatment agent is composed of the following raw materials in parts by weight: 0.2 parts of triethylamine, 7 parts of silica aerogel, 140 parts of calcium zeolite, 1.3 parts of ammonium persulfate, 7 parts of glycidyl methacrylate, 4 parts of aminosilane coupling agent and 50 parts of acrylamide.
The aminosilane coupling agent is a silane coupling agent kh550.
The preparation method of the silica aerogel doped calcium zeolite water treatment agent comprises the following steps:
(1) adding ammonium persulfate into deionized water with the weight 30 times that of the ammonium persulfate, and uniformly stirring;
(2) taking the calcium zeolite, sending the calcium zeolite into sodium hydroxide with the concentration of 1mol/l, soaking for 2 hours, discharging, calcining for 2 hours at 700 ℃, cooling, grinding into fine powder, mixing with glycidyl methacrylate, adding the mixture into deionized water with the weight 5 times that of the mixture, and stirring for 4 hours at 90 ℃ to obtain calcium zeolite dispersion liquid;
(3) mixing the silicon dioxide aerogel and the aminosilane coupling agent, adding the mixture into absolute ethyl alcohol which is 8 times of the weight of the mixture, raising the temperature to 65 ℃, keeping the temperature and stirring for 2 hours, and distilling to remove the ethyl alcohol to obtain the amino silicon dioxide aerogel;
(4) adding the amino silica aerogel into the calcium zeolite dispersion liquid, uniformly stirring, raising the temperature to 190 ℃, adding triethylamine, and stirring for 7 hours under heat preservation to obtain a modified calcium zeolite dispersion liquid;
(5) And adding acrylamide into the modified calcium zeolite dispersion liquid, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 75 ℃, adding the ammonium persulfate aqueous solution, preserving heat, stirring for 5 hours, discharging, carrying out suction filtration, washing a filter cake, drying at the temperature of 60 ℃ in vacuum for 4 hours, and cooling to normal temperature to obtain the silica aerogel doped calcium zeolite water treatment agent.
Example 2
A silica aerogel doped calcium zeolite water treatment agent is composed of the following raw materials in parts by weight: 0.1 part of triethylamine, 5 parts of silica aerogel, 100 parts of calcium zeolite, 1 part of ammonium persulfate, 5 parts of glycidyl methacrylate, 3 parts of aminosilane coupling agent and 40 parts of acrylamide.
The aminosilane coupling agent is a silane coupling agent kh550.
The preparation method of the silica aerogel doped calcium zeolite water treatment agent comprises the following steps:
(1) adding ammonium persulfate into deionized water with the weight of 20 times of that of the ammonium persulfate, and uniformly stirring;
(2) taking the calcium zeolite, sending the calcium zeolite into sodium hydroxide with the concentration of 0.8mol/l, soaking for 1 hour, discharging, calcining for 1 hour at the temperature of 600 ℃, cooling, grinding into fine powder, mixing with glycidyl methacrylate, adding the mixture into deionized water with the weight 3 times that of the mixture, and stirring for 2 hours at the temperature of 80 ℃ to obtain calcium zeolite dispersion liquid;
(3) Mixing the silicon dioxide aerogel and the aminosilane coupling agent, adding the mixture into absolute ethyl alcohol with the weight 6 times of that of the mixture, raising the temperature to 60 ℃, keeping the temperature and stirring for 1 hour, and distilling to remove the ethyl alcohol to obtain the amino silicon dioxide aerogel;
(4) adding the amino silica aerogel into the calcium zeolite dispersion liquid, uniformly stirring, raising the temperature to 170 ℃, adding triethylamine, and stirring for 4 hours under heat preservation to obtain a modified calcium zeolite dispersion liquid;
(5) and adding acrylamide into the modified calcium zeolite dispersion liquid, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 60 ℃, adding the ammonium persulfate aqueous solution, preserving heat, stirring for 3 hours, discharging, carrying out suction filtration, washing a filter cake, drying for 2 hours at the temperature of 50 ℃ in vacuum, and cooling to normal temperature to obtain the silica aerogel doped calcium zeolite water treatment agent.
Testing the performance;
heavy metal treatment test:
at pH 6, for Cu2+The adsorption capacity of (A) is: 231-240 mg/g;
at pH 3, for Cr6+The adsorption capacity of (A) is: 101-126 mg/g;
and (3) treatment and test of dye sewage:
the adsorption capacity to dye sewage is 1350-;
And (3) testing the treatment of the organic matter polluted water:
water treatment test for engine oil contamination: the adsorption weight of the lubricating oil can reach 40-45 times of the self weight.
Claims (2)
1. The silica aerogel doped calcium zeolite water treatment agent is characterized by being prepared from the following raw materials in parts by weight:
0.1-0.2 part of triethylamine, 5-7 parts of silica aerogel, 100 parts of calcium zeolite, 140 parts of ammonium persulfate, 1-1.3 parts of glycidyl methacrylate, 3-4 parts of aminosilane coupling agent and 40-50 parts of acrylamide;
the preparation method of the silica aerogel doped calcium zeolite water treatment agent comprises the following steps:
(1) adding ammonium persulfate into deionized water with the weight of 20-30 times of that of the ammonium persulfate, and uniformly stirring;
(2) taking the calcium zeolite, sending the calcium zeolite into sodium hydroxide with the concentration of 0.8-1mol/l, soaking for 1-2 hours, discharging, calcining for 1-2 hours at the temperature of 600-700 ℃, cooling, grinding into fine powder, mixing with glycidyl methacrylate, adding into deionized water with the weight of 3-5 times of that of the mixture, and stirring for 2-4 hours at the temperature of 80-90 ℃ to obtain calcium zeolite dispersion liquid;
(3) mixing the silicon dioxide aerogel and the aminosilane coupling agent, adding the mixture into absolute ethyl alcohol with the weight 6-8 times of that of the mixture, raising the temperature to 60-65 ℃, keeping the temperature, stirring for 1-2 hours, and distilling to remove the ethyl alcohol to obtain the amino silicon dioxide aerogel;
(4) Adding the amino silica aerogel into the calcium zeolite dispersion liquid, uniformly stirring, raising the temperature to be 170-190 ℃, adding triethylamine, and stirring for 4-7 hours under the condition of heat preservation to obtain a modified calcium zeolite dispersion liquid;
(5) adding acrylamide into the modified calcium zeolite dispersion liquid, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to be 60-75 ℃, adding the ammonium persulfate aqueous solution, keeping the temperature and stirring for 3-5 hours, discharging, performing suction filtration, washing a filter cake, drying for 2-4 hours at the temperature of 50-60 ℃ in vacuum, and cooling to normal temperature to obtain the silica aerogel doped calcium zeolite water treatment agent.
2. The silica aerogel-doped calcia zeolite water treatment agent as claimed in claim 1, wherein said aminosilane coupling agent is silane coupling agent kh 550.
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| CN108751372B true CN108751372B (en) | 2021-10-08 |
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| CN109464995A (en) * | 2018-12-06 | 2019-03-15 | 朱莲华 | A kind of graphene dopant dye Wastewater purification material and preparation method thereof |
| CN109607721A (en) * | 2018-12-27 | 2019-04-12 | 广东平润建设工程有限公司 | Black and odorous water administering method |
| CN110128905A (en) * | 2019-05-30 | 2019-08-16 | 黎明职业大学 | A kind of fiber base decorative material for wall surface |
| CN114672192B (en) * | 2022-05-20 | 2023-01-03 | 苏州中亚油墨有限公司 | High-fluidity high-adhesion-fastness gravure printing ink and preparation method thereof |
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Effective date of registration: 20240315 Address after: 400000, Group 1, Dalongju Committee, Shuijiang Town, Nanchuan District, Chongqing Patentee after: Chongqing Jiangnan Chemical Technology Co.,Ltd. Country or region after: China Address before: Room 1103-02, Gangcheng Plaza, No. 16, North Ring Road, economic and Technological Development Zone, Suzhou, Jiangsu 215400 Patentee before: Suzhou yanrongyu Technology Development Co.,Ltd. Country or region before: China |