CN113772760B - Water treatment agent used in perfume production process and preparation method thereof - Google Patents
Water treatment agent used in perfume production process and preparation method thereof Download PDFInfo
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- CN113772760B CN113772760B CN202111117051.9A CN202111117051A CN113772760B CN 113772760 B CN113772760 B CN 113772760B CN 202111117051 A CN202111117051 A CN 202111117051A CN 113772760 B CN113772760 B CN 113772760B
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- 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
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- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
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Abstract
The invention relates to a water treatment agent used in the production process of spices and a preparation method thereof, belonging to the technical field of water treatment agents, wherein the water treatment agent is prepared by the following steps: mixing iron-based montmorillonite with deionized water, adding modified cyclodextrin, and stirring for reaction for 24h to obtain a water treatment agent used in the perfume production process; because the synthetic perfume wastewater contains a large amount of organic matters which have toxic action on microorganisms and are difficult to degrade, and the synthetic perfume wastewater lacks of nutrient elements, the effect of directly treating the wastewater by a biochemical method is extremely low, and sometimes even the wastewater cannot be operated. Through chemical oxidation, a plurality of toxic, harmful and nondegradable organic matters in the wastewater can be converted into substances which are slightly toxic, nontoxic and easily degradable.
Description
Technical Field
The invention belongs to the technical field of water treatment agents, and particularly relates to a water treatment agent used in a perfume production process and a preparation method thereof.
Background
The perfume is closely related to the life of people, the perfume industry develops rapidly in the last decade, thousands of enterprises with hundreds of billions of annual output values bring about increasingly serious environmental protection problems, the perfume wastewater has complex and variable components, some wastewater has high organic matter concentration, is difficult to biodegrade, has high acidity and alkalinity and salt content, contains oil or surfactant and the like, and has great treatment difficulty. The organic components of the waste water contain a large amount of aromatic hydrocarbon, aromatic compounds and derivatives thereof, more than twenty, and the organic components also comprise substances which have the inhibiting effect on the growth of microorganisms, such as phenol, toluene, benzaldehyde and the like; a large amount of surfactant is added in the process of washing a reaction kettle and the like, so that the wastewater has the characteristics of high concentration, large water quality fluctuation, containing a large amount of organic substances with the effect of inhibiting the growth of microorganisms and complex pollution source components in water.
Disclosure of Invention
In order to solve the technical problems mentioned in the background technology, the invention provides a water treatment agent used in the production process of spices and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
because the synthetic perfume wastewater contains a large amount of organic matters which have toxic action on microorganisms and are difficult to degrade, and the synthetic perfume wastewater lacks of nutrient elements, the effect of directly treating the wastewater by a biochemical method is extremely low, and sometimes even the wastewater cannot be operated. Through chemical oxidation, a plurality of toxic, harmful and nondegradable organic matters in the wastewater can be converted into substances which are slightly toxic, nontoxic and easily degradable.
A preparation method of a water treatment agent used in a perfume production process comprises the following steps:
mixing iron-based montmorillonite with deionized water, adding modified cyclodextrin, stirring and reacting for 24 hours at 20-30 ℃, adjusting the pH value to 7 by using a hydrochloric acid solution after the reaction is finished, then carrying out vacuum filtration, washing a filter cake for three times by using distilled water, and carrying out vacuum drying at 60 ℃ after the washing is finished to constant weight, thereby obtaining the water treatment agent used in the perfume production process. The iron-based montmorillonite and the modified cyclodextrin are subjected to ion exchange, wherein the modified cyclodextrin contains a quaternary ammonium salt structure, the modified cyclodextrin is immobilized on the surface of the iron-based montmorillonite, the cyclodextrin is a natural polymer with a special pore structure, and the outer edge of the cyclodextrin contains a large number of hydroxyl groups to present hydrophilicity, while the inner cavity presents hydrophobicity. The inner cavity can perform inclusion with organic matters to reduce the concentration of the organic matters.
Further, the dosage ratio of the iron-based montmorillonite, the modified cyclodextrin and the deionized water is 5-8g:1-2g:50mL.
Further, the modified cyclodextrin is prepared by the following steps:
s11, under the protection of nitrogen and at the temperature of 0 ℃, mixing beta-cyclodextrin and N, N-dimethylformamide, adding octenyl succinic anhydride, stirring for 10min, then heating to 80 ℃, stirring for 9h, cooling to room temperature after the reaction is finished, adding trichloromethane with three times of volume, filtering, washing a filter cake with acetone, and drying at the temperature of 60 ℃ to constant weight after the washing is finished to obtain a solid a;
and S12, under the condition of nitrogen protection, adding the solid a and a modifier into deionized water, stirring for dissolving, then adding an initiator, stirring for reacting for 9 hours at 65 ℃, cooling to room temperature after the reaction is finished, then mixing with acetone with twice the volume, carrying out vacuum filtration, and drying a filter cake to constant weight at 60 ℃ to obtain the modified cyclodextrin.
Further, in step S11, the amount ratio of β -cyclodextrin, octenyl succinic anhydride, and N, N-dimethylformamide was 5g:2g:50mL; in the step S12, the initiator is ammonium persulfate, sodium bisulfite and deionized water according to the dosage ratio of 0.01mol:0.01mol:20mL of the mixture is mixed; the dosage ratio of the solid a, the modifier, the deionized water and the initiator is 5.5g:1.8g:50mL of: 1mL.
Further, the modifier is prepared by the following steps:
mixing dimethylamino ethyl methacrylate and 2- (2 ' -hydroxy-3 ',5' -di-tert-butylphenyl) -5-chlorobenzotriazole, adding acetonitrile, reacting under stirring at 45 ℃ for 12 hours, then freezing and crystallizing, washing the obtained crystal with diethyl ether, and then drying in vacuum to constant weight to obtain the modifier.
The reaction process is as follows:
further, the molar ratio of the used dimethylaminoethyl methacrylate to the 2- (2 ' -hydroxy-3 ',5' -di-tert-butylphenyl) -5-chlorobenzotriazole is 1.1:1; the dosage ratio of the dimethylaminoethyl methacrylate to the acetonitrile is 1g:10mL.
Further, the iron-based montmorillonite is prepared by the following steps:
mixing sodium-based montmorillonite and deionized water, stirring for 2h at the temperature of 30 ℃, then adding an iron chloride solution, stirring for 6h, centrifugally separating and washing after stirring is finished, and washing until the washing liquid does not contain chloride ions, thereby obtaining the iron-based montmorillonite. The iron-based montmorillonite is matched with the modified cyclodextrin to improve the photo-Fenton catalytic activity, the iron-based montmorillonite has the advantages of large specific surface area and good stability, and the ultraviolet absorption structure in the modified cyclodextrin improves the stability of a water treatment agent and promotes the catalytic efficiency.
Further, the dosage ratio of the sodium montmorillonite, the deionized water and the ferric chloride solution is 5g:200mL of: 100mL; the ferric chloride solution is ferric chloride hexahydrate and deionized water according to the dosage ratio of 5g:100mL of the mixture is mixed.
The invention has the beneficial effects that:
the invention discloses a water treatment agent used in the perfume production process, which carries iron element and modified cyclodextrin on the surface of montmorillonite to carry out oxidative degradation on perfume wastewater, so that part of organic matters which are difficult to degrade are oxidized and decomposed, the toxicity is reduced, and the biodegradability of the wastewater is improved. The modified cyclodextrin takes an ultraviolet absorbent as a raw material, 2- (2 ' -hydroxy-3 ',5' -di-tert-butylphenyl) -5-chlorobenzotriazole reacts with dimethylaminoethyl methacrylate to prepare the modifier containing an unsaturated quaternary ammonium salt structure, the modifier is firstly subjected to polymerization reaction with beta-cyclodextrin and then subjected to ion exchange with iron-based montmorillonite to modify the ultraviolet absorption structure in the cyclodextrin, so that the stability of a water treatment agent is improved, and the catalytic efficiency is promoted.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing a modifier:
mixing dimethylaminoethyl methacrylate and 2- (2 ' -hydroxy-3 ',5' -di-tert-butylphenyl) -5-chlorobenzotriazole, adding acetonitrile, stirring and reacting at 45 ℃ for 12h, then freezing and crystallizing, washing the obtained crystal with diethyl ether, and then drying in vacuum to constant weight to obtain a modifier; wherein the dosage molar ratio of the dimethylamino ethyl methacrylate to the 2- (2 ' -hydroxy-3 ',5' -di-tert-butylphenyl) -5-chlorobenzotriazole is 1.1:1; the dosage ratio of the dimethylaminoethyl methacrylate to the acetonitrile is 1g:10mL.
Example 2
Further, the modified cyclodextrin is prepared by the following steps:
s11, under the protection of nitrogen and at the temperature of 0 ℃, mixing beta-cyclodextrin and N, N-dimethylformamide, adding octenyl succinic anhydride, stirring for 10min, then heating to 80 ℃, stirring for 9h, cooling to room temperature after the reaction is finished, adding trichloromethane with three times of volume, filtering, washing a filter cake with acetone, and drying at the temperature of 60 ℃ to constant weight after the washing is finished to obtain a solid a; wherein the dosage ratio of the beta-cyclodextrin to the octenyl succinic anhydride to the N, N-dimethylformamide is 5g:2g:50mL;
s12, under the protection of nitrogen, adding the solid a and a modifier into deionized water, stirring for dissolving, then adding an initiator, stirring for reacting for 9 hours at 65 ℃, cooling to room temperature after the reaction is finished, then mixing with acetone with twice the volume, carrying out vacuum filtration, drying a filter cake to constant weight at 60 ℃, and obtaining modified cyclodextrin; wherein the initiator is ammonium persulfate, sodium bisulfite and deionized water according to the dosage ratio of 0.01mol:0.01mol:20mL of the mixture is mixed; the dosage ratio of the solid a, the modifier, the deionized water and the initiator is 5.5g:1.8g:50mL of: 1mL; the modifier was prepared as in example 1.
Example 3
Preparing iron-based montmorillonite:
mixing sodium-based montmorillonite and deionized water, stirring for 2h at the temperature of 30 ℃, then adding an iron chloride solution, stirring for 6h, centrifugally separating and washing after stirring is finished, and washing until the washing liquid does not contain chloride ions to obtain iron-based montmorillonite; wherein the dosage ratio of the sodium-based montmorillonite, the deionized water and the ferric chloride solution is 5g:200mL of the solution: 100mL; the ferric chloride solution is ferric trichloride hexahydrate and deionized water according to the dosage ratio of 5g:100mL of the mixture is mixed.
Example 4
A preparation method of a water treatment agent used in a perfume production process comprises the following steps:
mixing iron-based montmorillonite and deionized water, adding modified cyclodextrin, stirring and reacting for 24 hours at 20 ℃, adjusting the pH value to 7 by using a hydrochloric acid solution after the reaction is finished, then carrying out vacuum filtration, washing a filter cake for three times by using distilled water, and carrying out vacuum drying to constant weight at 60 ℃ after the washing is finished, thereby obtaining the water treatment agent used in the perfume production process.
Wherein the dosage ratio of the iron-based montmorillonite, the modified cyclodextrin and the deionized water is 5g:1g:50mL; iron-based montmorillonite was prepared as in example 3; modified cyclodextrin was prepared as in example 2.
Example 5
A preparation method of a water treatment agent used in a perfume production process comprises the following steps:
mixing iron-based montmorillonite with deionized water, adding modified cyclodextrin, stirring and reacting for 24 hours at 25 ℃, adjusting the pH value to 7 by using a hydrochloric acid solution after the reaction is finished, then carrying out vacuum filtration, washing a filter cake for three times by using distilled water, and carrying out vacuum drying to constant weight at 60 ℃ after the washing is finished, thereby obtaining the water treatment agent used in the perfume production process.
Wherein the dosage ratio of the iron-based montmorillonite, the modified cyclodextrin and the deionized water is 6g:1.5g:50mL; iron-based montmorillonite was prepared as in example 3; modified cyclodextrin was prepared as in example 2.
Example 6
A preparation method of a water treatment agent used in a perfume production process comprises the following steps:
mixing iron-based montmorillonite and deionized water, adding modified cyclodextrin, stirring and reacting for 24 hours at 30 ℃, adjusting the pH value to 7 by using a hydrochloric acid solution after the reaction is finished, then carrying out vacuum filtration, washing a filter cake for three times by using distilled water, and carrying out vacuum drying to constant weight at 60 ℃ after the washing is finished, thereby obtaining the water treatment agent used in the perfume production process.
Wherein the dosage ratio of the iron-based montmorillonite, the modified cyclodextrin and the deionized water is 8g:2g:50mL; iron-based montmorillonite was prepared as in example 3; modified cyclodextrin was prepared as in example 2.
Comparative example 1
The modified cyclodextrin in example 2 was replaced with beta-cyclodextrin, and the remaining raw materials and preparation process remained unchanged.
Comparative example 2
The iron-based montmorillonite in example 2 was replaced with sodium-based montmorillonite, and the remaining raw materials and preparation process remained unchanged.
The samples obtained in examples 4 to 6 and comparative examples 1 to 2 were subjected to the test;
taking 1000mL of perfume water sample in a beaker, simultaneously placing the beaker on a small-sized magnetic stirrer, and using H 2 SO 4 Or NaOH is used for adjusting the pH value to 3, and the prepared sample is added while stirring; the adding amount of the sample is 4g/L; after the above operation is completed, a certain volume of H is added 2 O 2 And simulating sunlight by using a 1000W xenon lamp as a light source, and taking 20mL of water sample from the beaker after reacting for 3 h. After each sample is taken, the pH value is measured, and then H is used 2 SO 4 Or NaOH is used for adjusting the pH value to be neutral, the precipitate is filtered, and 10mL of filtered water sample is taken for measuring COD;
the test results are shown in table 1 below:
TABLE 1
As can be seen from the above Table 1, the water treatment agent prepared by the invention has the advantages of small investment, fast reaction and obvious effect when used for treating the perfume and perfume wastewater.
In the description of the specification, reference to the description of "one embodiment," "an example," "a specific example" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only, and it will be appreciated by those skilled in the art that various modifications, additions and substitutions can be made to the embodiments described without departing from the scope of the invention as defined in the appended claims.
Claims (6)
1. A preparation method of a water treatment agent used in a perfume production process is characterized by comprising the following steps:
mixing iron-based montmorillonite with deionized water, adding modified cyclodextrin, and stirring and reacting at 20-30 ℃ for 24h to obtain a water treatment agent used in the perfume production process;
the modified cyclodextrin is prepared by the following steps:
s11, under the protection of nitrogen and at the temperature of 0 ℃, mixing beta-cyclodextrin and N, N-dimethylformamide, adding octenyl succinic anhydride, stirring for 10min, then heating to 80 ℃, and stirring for 9h to obtain a solid a;
step S12, mixing dimethylamino ethyl methacrylate and 2- (2 ' -hydroxy-3 ',5' -di-tert-butylphenyl) -5-chlorobenzotriazole, adding acetonitrile, and reacting under stirring at 45 ℃ for 12 hours to obtain a modifier; and under the protection of nitrogen, adding the solid a and a modifier into deionized water, stirring for dissolving, then adding an initiator, and stirring for reacting for 9 hours at 65 ℃ to obtain the modified cyclodextrin.
2. The method according to claim 1, wherein in the step of mixing iron-based montmorillonite with deionized water and then adding modified cyclodextrin, the amount ratio of iron-based montmorillonite to modified cyclodextrin to deionized water is 5-8g:1-2g:50mL.
3. The method of claim 1, wherein the amount ratio of β -cyclodextrin, octenyl succinic anhydride and N, N-dimethylformamide used in step S11 is 5g:2g:50mL; in the step S12, the initiator is ammonium persulfate, sodium bisulfite and deionized water according to the dosage ratio of 0.01mol:0.01mol:20mL of the mixture is mixed; step S12 the dosage ratio of the solid a, the modifier, the deionized water and the initiator is 5.5g:1.8g:50mL of: 1mL.
4. The method according to claim 1, wherein the molar ratio of the amount of dimethylaminoethyl methacrylate to the amount of 2- (2 ' -hydroxy-3 ',5' -di-tert-butylphenyl) -5-chlorobenzotriazole used is 1.1:1; the dosage ratio of the dimethylaminoethyl methacrylate to the acetonitrile is 1g:10mL.
5. The method of claim 1, wherein the iron-based montmorillonite is prepared by the steps of:
mixing sodium-based montmorillonite and deionized water, stirring for 2h at the temperature of 30 ℃, then adding an iron chloride solution, stirring for 6h, centrifugally separating and washing after stirring is finished, and washing until the washing liquid does not contain chloride ions, thereby obtaining the iron-based montmorillonite.
6. A water treatment agent for use in a perfume production process, characterized by being prepared by the preparation method of claim 1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111117051.9A CN113772760B (en) | 2021-09-23 | 2021-09-23 | Water treatment agent used in perfume production process and preparation method thereof |
| PCT/CN2022/110549 WO2023045594A1 (en) | 2021-09-23 | 2022-08-05 | Water treatment agent used in perfume production process and preparation method therefor |
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| CN202111117051.9A CN113772760B (en) | 2021-09-23 | 2021-09-23 | Water treatment agent used in perfume production process and preparation method thereof |
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| CN113772760B true CN113772760B (en) | 2022-12-27 |
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| CN113772760B (en) * | 2021-09-23 | 2022-12-27 | 安徽华业香料股份有限公司 | Water treatment agent used in perfume production process and preparation method thereof |
| CN117623426B (en) * | 2024-01-25 | 2024-04-12 | 山东道简环保科技有限公司 | Preparation method of sewage treatment medicament |
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| JPS62191416A (en) * | 1986-02-14 | 1987-08-21 | Natl Inst For Res In Inorg Mater | Montmorillonite-methylated cyclodextrin-type crystalline composite and production thereof |
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| CN107935098A (en) * | 2017-12-25 | 2018-04-20 | 芜湖皖江知识产权运营中心有限公司 | A kind of method for handling organic wastewater |
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| CN101177310B (en) * | 2007-11-02 | 2010-05-19 | 西南石油大学 | Method for preparing waste-water treating agent containing organic dye |
| US8673272B2 (en) * | 2009-07-27 | 2014-03-18 | Isp Investments Inc. | Ultraviolet-absorbing compounds |
| JP2013000696A (en) * | 2011-06-20 | 2013-01-07 | Fujifilm Corp | Water purification method |
| CN110734180A (en) * | 2019-10-16 | 2020-01-31 | 利安隆科润(浙江)新材料有限公司 | method for recycling and applying catalytic hydrogenation method to prepare alkaline water in ultraviolet absorbent reaction liquid |
| CN112958090B (en) * | 2021-02-05 | 2023-05-12 | 长春工业大学 | Efficient and stable iron-copper montmorillonite heterogeneous Fenton catalyst and preparation method and application thereof |
| CN113772760B (en) * | 2021-09-23 | 2022-12-27 | 安徽华业香料股份有限公司 | Water treatment agent used in perfume production process and preparation method thereof |
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- 2021-09-23 CN CN202111117051.9A patent/CN113772760B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS62191416A (en) * | 1986-02-14 | 1987-08-21 | Natl Inst For Res In Inorg Mater | Montmorillonite-methylated cyclodextrin-type crystalline composite and production thereof |
| CN101774676A (en) * | 2010-01-20 | 2010-07-14 | 华东理工大学 | Method for treating high-concentration industrial organic waste water and relevant catalyst |
| CN102503017A (en) * | 2011-11-09 | 2012-06-20 | 广西博世科环保科技股份有限公司 | Method for treating non-degradable organic wastewater by multielement multiphase membrane technology |
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