CN115159651B - Preparation process of sewage treatment agent - Google Patents
Preparation process of sewage treatment agent Download PDFInfo
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- CN115159651B CN115159651B CN202210885043.7A CN202210885043A CN115159651B CN 115159651 B CN115159651 B CN 115159651B CN 202210885043 A CN202210885043 A CN 202210885043A CN 115159651 B CN115159651 B CN 115159651B
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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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Removal Of Specific Substances (AREA)
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Abstract
The invention discloses a preparation process of a sewage treatment agent, which comprises the steps of dissolving cellulose in an alkaline solution to prepare a solution I, and dissolving citric acid in distilled water to prepare a solution II; mixing the solution I and the solution II, and preparing gel by adopting a freeze thawing method; crystallizing the gel obtained in the step S2 at a low temperature to obtain cellulose crystals; dispersing starch in distilled water, continuously stirring, adding starch xanthate and cellulose crystal, adding tween for emulsification, freeze drying, and grinding to obtain the sewage treatment agent.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to a preparation process of a sewage treatment agent.
Background
In recent years, with the continuous progress of industrialization, environmental pollution problems caused by industry are becoming serious, especially for water resources, soil and air. There are also many researchers that have begun to investigate how to alleviate the problems of water pollution and the like. At present, three common methods for treating heavy metal wastewater are as follows: the method for removing heavy metal ions in wastewater through chemical reaction comprises a neutralization precipitation method, a sulfide precipitation method, a ferrite coprecipitation method, a chemical reduction method, an electrochemical reduction method, a high molecular heavy metal trapping agent method and the like; the second category is a method for adsorbing, concentrating and separating heavy metals in wastewater under the condition of not changing the chemical form of the heavy metals, and the method comprises adsorption, solvent extraction, evaporation and solidification methods, ion exchange, membrane separation and the like. The third category is a method for removing heavy metals from wastewater by flocculation, absorption, accumulation, enrichment and the like of microorganisms or plants, wherein the method comprises biological flocculation, biochemical method, ecological restoration of plants and the like.
Chinese patent document CN111689589a discloses a sewage treatment agent, comprising the following raw materials: organic carboxylic acid, modified sisal fiber porous microspheres, polyamino acid, starch xanthate and aminotrimethylene phosphonic acid. After the experiment example tests, the wastewater treatment agent has the removal rates of cadmium, lead, copper, nickel and zinc in heavy metal wastewater of more than 99.9%, more than 99.4%, more than 99.3%, more than 99.8% and more than 99.3%, and the removal rates of chromium, manganese and mercury in heavy metal wastewater of more than 99.7%, more than 99.9% and more than 99.9%, respectively, so that the treatment effect is good.
Disclosure of Invention
Aiming at the prior art that the sewage treatment agent is prepared by simply mixing raw materials, the acid radical ions which play a role in removing metal ions and the preferential sequence of forming coordination by the metal ions are different in the sewage treatment process, so that the metal removing effect of easily forming coordination bonds is good, and the metal ion removing effect of difficultly forming coordination bonds is poor.
The invention aims to provide a preparation process of a sewage treatment agent, which comprises the following steps of:
s1: cellulose is dissolved in an alkaline solution to prepare a solution I, and citric acid is dissolved in distilled water to prepare a solution II.
S2: and mixing the solution I and the solution II, and preparing gel by adopting a freeze thawing method.
S3: and (3) crystallizing the cellulose gel at a low temperature by using the gel obtained in the step (S2) to obtain cellulose crystals.
S4: dispersing starch in distilled water, continuously stirring, adding starch xanthate and cellulose crystal, adding tween for emulsification, freeze drying, and grinding to obtain the sewage treatment agent.
Further, the solution I prepared by dissolving cellulose in alkaline solution is prepared by mixing, stirring and standing cellulose, urea and alkaline solution at-3 to-8 ℃ for 20-30 min, taking out, stirring at room temperature for 5-10 min, and then standing in the temperature environment for 3-6 times repeatedly.
Further, the alkaline solution is sodium hydroxide solution or potassium hydroxide solution with the mass concentration of 28-35%.
Still further, the mass ratio of the cellulose, the urea and the alkaline solution is (1-2): (0.75-0.94): (3-6).
Further, the temperature of the gel prepared by the freeze thawing method is between-2 ℃ and-8 ℃, and the freeze thawing time is 3-10 h.
Further, the temperature of the cellulose crystallization at the low temperature is between-20 ℃ and-30 ℃ and the time is between 10h and 30h.
Further, the Tween is any one of Tween-20, tween-40, tween-60 or Tween-80.
Further, the temperature of emulsification in the step S4 is 35-50 ℃ and the time is 5-16 h.
Further, the mass ratio of the starch, the starch xanthate and the cellulose crystal is (1-2): (0.6-0.9): (0.45-0.88).
The invention also has the following beneficial effects:
1. according to the invention, cellulose spherulites are prepared by adopting cellulose, wherein citric acid is easy to form a complex to enter the cellulose spherulites pore canal, and the prepared sewage treatment agent has a complexing effect when metal ions enter the pore canal in the sewage treatment process, and the complexing effect does not carry out priority selection on the metal ions, so that the sewage treatment agent has a good effect of removing the metal ions.
2. According to the invention, cellulose spherulites and starch xanthate are dispersed in a starch solution, starch is coated on the surface of the spherulites after tween fermentation, and simultaneously, the starch xanthate is coated in the spherulites and starch intermediate-grade spherulites pore canals, and the starch xanthate is easy to form a complex with heavy metal ions at normal temperature, so that metal ions can form complexation with metal ions after entering from starch gaps when the treating agent is used for treating sewage, and an excellent sewage treatment effect is achieved.
3. In the invention, the surfaces of the cellulose spherulites and the starch contain rich hydroxyl groups, and the cellulose spherulites and the starch form hydrogen bond action with metal ions, so that the effect of removing the metal ions is excellent, and meanwhile, the hydrogen bond action is relatively easy to break, so that the treating agent can be desorbed and applied for the second time.
Drawings
FIG. 1 is a preparation process diagram of the sewage treatment agent of the invention.
Detailed Description
The following detailed description of the embodiments of the present invention is provided on the premise of the technical solution of the present invention, and the detailed implementation manner and specific operation process are provided, and it should be noted that, for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered as the protection scope of the present invention.
Example 1
The preparation process of the sewage treatment agent specifically comprises the following steps:
s1: cellulose is dissolved in an alkaline solution to prepare a solution I, and citric acid is dissolved in distilled water to prepare a solution II.
S2: and mixing the solution I and the solution II, and preparing gel by adopting a freeze thawing method.
S3: and (3) crystallizing the cellulose gel at a low temperature by using the gel obtained in the step (S2) to obtain cellulose crystals.
S4: dispersing starch in distilled water, continuously stirring, adding starch xanthate and cellulose crystal, adding tween for emulsification, freeze drying, and grinding to obtain the sewage treatment agent.
The solution I prepared by dissolving cellulose in alkaline solution is prepared by mixing cellulose, urea and alkaline solution, stirring, standing at-3deg.C for 20min, taking out, stirring at room temperature for 5min, standing in the above temperature environment, and repeating for 3 times; the alkaline solution is sodium hydroxide solution with the mass concentration of 28%; the mass ratio of cellulose to urea to alkaline solution is 1:0.75:3, a step of; the temperature for preparing gel by the freeze thawing method is between-2 ℃ and the freeze thawing time is 3 hours; the temperature of cellulose crystallization at the low temperature is-20 ℃ and the time is 10 hours; the Tween is Tween-20; the temperature of emulsification in the step S4 is 35 ℃ and the time is 5 hours; the mass ratio of the starch to the starch xanthate to the cellulose crystal is 1:0.6:0.45.
example 2
The preparation process of the sewage treatment agent specifically comprises the following steps:
s1: cellulose is dissolved in an alkaline solution to prepare a solution I, and citric acid is dissolved in distilled water to prepare a solution II.
S2: and mixing the solution I and the solution II, and preparing gel by adopting a freeze thawing method.
S3: and (3) crystallizing the cellulose gel at a low temperature by using the gel obtained in the step (S2) to obtain cellulose crystals.
S4: dispersing starch in distilled water, continuously stirring, adding starch xanthate and cellulose crystal, adding tween for emulsification, freeze drying, and grinding to obtain the sewage treatment agent.
The solution I prepared by dissolving cellulose in alkaline solution is prepared by mixing cellulose, urea and alkaline solution, stirring, standing at-8deg.C for 30min, taking out, stirring at room temperature for 10min, standing in the above temperature environment, and repeating for 6 times; the alkaline solution is a potassium hydroxide solution with the mass concentration of 35%; the mass ratio of cellulose to urea to alkaline solution is 2:0.94:6, preparing a base material; the temperature for preparing gel by the freeze thawing method is between-8 ℃ and the freeze thawing time is 10 hours; the temperature of cellulose crystallization at the low temperature is minus 30 ℃ and the time is 30 hours; the Tween is Tween-40; the temperature of emulsification in the step S4 is 50 ℃ and the time is 16 hours; the mass ratio of the starch to the starch xanthate to the cellulose crystal is 2:0.9:0.88.
example 3
The preparation process of the sewage treatment agent specifically comprises the following steps:
s1: cellulose is dissolved in an alkaline solution to prepare a solution I, and citric acid is dissolved in distilled water to prepare a solution II.
S2: and mixing the solution I and the solution II, and preparing gel by adopting a freeze thawing method.
S3: and (3) crystallizing the cellulose gel at a low temperature by using the gel obtained in the step (S2) to obtain cellulose crystals.
S4: dispersing starch in distilled water, continuously stirring, adding starch xanthate and cellulose crystal, adding tween for emulsification, freeze drying, and grinding to obtain the sewage treatment agent.
The solution I prepared by dissolving cellulose in alkaline solution is prepared by mixing cellulose, urea and alkaline solution, stirring, standing at-5deg.C for 25min, taking out, stirring at room temperature for 7min, standing in the above temperature environment, and repeating for 4 times; the alkaline solution is a potassium hydroxide solution with the mass concentration of 30%; the mass ratio of cellulose, urea and alkaline solution is 1.4:0.82:4, a step of; the temperature for preparing gel by the freeze thawing method is-4 ℃, and the freeze thawing time is 5 hours; the temperature of cellulose crystallization at the low temperature is-25 ℃ and the time is 14 hours; the Tween is Tween-60; the temperature of emulsification in the step S4 is 40 ℃ and the time is 10 hours; the mass ratio of the starch to the starch xanthate to the cellulose crystal is 1.8:0.7:0.56.
example 4
The preparation process of the sewage treatment agent specifically comprises the following steps:
s1: cellulose is dissolved in an alkaline solution to prepare a solution I, and citric acid is dissolved in distilled water to prepare a solution II.
S2: and mixing the solution I and the solution II, and preparing gel by adopting a freeze thawing method.
S3: and (3) crystallizing the cellulose gel at a low temperature by using the gel obtained in the step (S2) to obtain cellulose crystals.
S4: dispersing starch in distilled water, continuously stirring, adding starch xanthate and cellulose crystal, adding tween for emulsification, freeze drying, and grinding to obtain the sewage treatment agent.
The solution I prepared by dissolving cellulose in alkaline solution is prepared by mixing cellulose, urea and alkaline solution, stirring, standing at-6deg.C for 28min, taking out, stirring at room temperature for 8min, standing in the above temperature environment, and repeating for 5 times; the alkaline solution is sodium hydroxide solution or potassium hydroxide solution with the mass concentration of 32%; the mass ratio of cellulose, urea and alkaline solution is 1.8:0.92:5, a step of; the temperature for preparing gel by the freeze thawing method is between-6 ℃ and the freeze thawing time is 9 hours; the temperature of cellulose crystallization at the low temperature is-27 ℃ and the time is 25 hours; the Tween is Tween-80; the temperature of emulsification in the step S4 is 45 ℃ and the time is 15 hours; the mass ratio of the starch to the starch xanthate to the cellulose crystal is 1.7:0.8:0.84.
performance test: the sewage treatment agents prepared in examples 1 to 4 were subjected to heavy metal sewage treatment, heavy metal sewage treatment water samples were prepared first, then the same amount of the treatment agents (50 mg) prepared in examples 1 to 4 were added respectively to treat for a certain period of time for detection, the results are shown in table 1,
table 1. Test results:
as can be seen from table 1, the treatment agents prepared in examples 1 to 4 have excellent removal rates of metal ions in sewage, and various metal ion mixed treatment agents can well remove mixed metal ions, and have excellent removal efficiency.
2. Preparing an equal amount (the content of each liter of water is 100 mg) of each metal ion sewage water sample (water samples 1-10), respectively treating the water samples with the treating agents prepared in examples 1-4, detecting after a period of treatment, and calculating the removal rate, wherein the removal rate is = (m) 0 -m 1 )÷m 0 ×100％，m 0 For initial metal ion content, m 1 For the removal of the post metal ion content, the results are shown in table 2,
table 2. Test results:
as can be seen from Table 2, the wastewater produced by using the wastewater treatment agents of examples 1 to 4 alone had the removal rate of 99% or more and the excellent removal rate of metal ions.
Claims (2)
1. The preparation process of the sewage treatment agent is characterized by comprising the following steps of:
s1: dissolving cellulose in an alkaline solution to prepare a solution I, and dissolving citric acid in distilled water to prepare a solution II; the alkaline solution is a sodium hydroxide solution or a potassium hydroxide solution with the mass concentration of 28-35%;
s2: mixing the solution I and the solution II, and preparing gel by adopting a freeze thawing method; the temperature for preparing gel by the freeze thawing method is between-2 and-8 ℃, and the freeze thawing time is 3-10 hours;
s3: crystallizing the gel obtained in the step S2 at a low temperature to obtain cellulose crystals; the crystallization temperature of the cellulose gel at the low temperature is-20 to-30 ℃ and the time is 10-30 hours;
s4: dispersing starch in distilled water, continuously stirring and adding starch xanthate and cellulose crystals, then adding tween for emulsification, freeze-drying and grinding to obtain a sewage treatment agent; wherein the temperature of the emulsification is 35-50 ℃ and the time is 5-16 h;
the cellulose is dissolved in an alkaline solution to prepare a solution I, the cellulose, urea and the alkaline solution are mixed, stirred and kept stand at-3 to-8 ℃ for 20-30 min, taken out, stirred at room temperature for 5-10 min, and then placed in the environment of-3 to-8 ℃ for 3-6 times repeatedly;
the mass ratio of the cellulose to the urea to the alkaline solution is (1-2): (0.75 to 0.94): (3-6);
the mass ratio of the starch to the starch xanthate to the cellulose crystal is (1-2): (0.6 to 0.9): (0.45-0.88).
2. The process for preparing a sewage treatment agent according to claim 1, wherein the tween is any one of tween-20, tween-40, tween-60 and tween-80.
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| CN202210885043.7A CN115159651B (en) | 2022-07-26 | 2022-07-26 | Preparation process of sewage treatment agent |
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| CN202210885043.7A CN115159651B (en) | 2022-07-26 | 2022-07-26 | Preparation process of sewage treatment agent |
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| CN115159651B true CN115159651B (en) | 2023-07-21 |
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Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3040855B2 (en) * | 1991-09-11 | 2000-05-15 | 旭化成工業株式会社 | Freezing stabilization method of cellulose aqueous dispersion |
| CN1453890A (en) * | 2003-04-28 | 2003-11-05 | 振华集团深圳电子有限公司 | Composite polycrystal oxide and its synthesis |
| CN105601755A (en) * | 2015-11-05 | 2016-05-25 | 深圳多元拓展环保科技有限公司 | Preparation method and application method of cellulose xanthogenate heavy metal capturing agent |
| CN109734145B (en) * | 2019-03-25 | 2022-06-21 | 新乡学院 | Composite flocculant for treating printing and dyeing wastewater |
| CN111689589A (en) * | 2020-05-28 | 2020-09-22 | 南京奥伯尔环保设备有限公司 | Sewage treatment agent |
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Effective date of registration: 20230703 Address after: 257000 No. 45, Liaohe Road, Dongying District, Dongying City, Shandong Province Applicant after: Dongying Dashun Chemical Co.,Ltd. Address before: No. 10, Group 6, Shangying Village, Fuxing Town, Zhongxian County, Chongqing 404300 Applicant before: Xie Liangya |
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