CN108516561B - Clay modification method suitable for preparation of harmful algal bloom prevention and control material - Google Patents
Clay modification method suitable for preparation of harmful algal bloom prevention and control material Download PDFInfo
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Abstract
The invention belongs to the field of harmful algal bloom prevention and control, and particularly relates to a preparation method of a harmful algal bloom prevention and control material. The method comprises the steps of taking natural clay mineral as a base material, crushing the natural clay mineral into powder clay, and then performing temperature-controlled roasting → acid activation → secondary addition neutralization → alkali neutralization → secondary addition mixing → temperature-controlled curing to realize composite treatment on the base material, thereby obtaining the modified clay with high-efficiency elimination capability on harmful algal bloom organisms. The composite treatment is preferably a one-pot method process, and is finished in a reaction pot by step-by-step treatment and flowing water. The method is suitable for clay mineral materials of different grades, and can prepare a harmful algal bloom remover which is more efficient than the existing method for synthesizing the modified clay; because the green natural clay mineral is used as the base material, no toxic and harmful pollutant or waste is generated in the treatment process, so that the processing process and the final product both meet the green environmental protection standard, and the high-efficiency comprehensive utilization of resources can be realized.
Description
Technical Field
The invention belongs to the field of harmful algal bloom prevention and control, and particularly relates to a preparation method of a harmful algal bloom prevention and control material.
Background
The method for preventing and treating the harmful algal blooms by the modified clay method is a method for improving the surface modification efficiency for overcoming the defects of low flocculation capacity, large using amount and the like of the natural clay minerals on the basis of fully utilizing the natural clay mineral method to treat the harmful algal blooms by scientists in China at the end of the last century, and then is developed gradually to form a set of method for efficiently removing the harmful algal blooms. Through the development of more than twenty years, the modified clay method has been developed into the most effective and feasible method for preventing and treating the harmful algal bloom at home and abroad at present, and has received extensive attention, research and application.
One of the key technologies for preventing and controlling harmful algal blooms by a modified clay method is to prepare a modified clay material with high-efficiency elimination capability on harmful algal bloom organisms. The disclosed technology and method generally introduces some compounds such as macromolecular flocculants, surfactants and the like with excellent flocculation effect into clay minerals to achieve the purpose of improving the flocculation algae removal capability of the clay, for example, Shu Shi Ming et al (1994) proposes to introduce macromolecular polyaluminum hydroxychloride into the clay to improve the algae removal efficiency of the clay by about 20 times; caochi Hua et al (2003) propose to introduce an organic surfactant cetyl trimethyl ammonium bromide into clay, and the amount of the obtained organically modified clay used for removing more than 95% of red tide algae is only 0.01 g/L. The processing and preparation of the modified clay materials are lack of targeted process research and development, and the reported preparation method has no exception that the modified clay is obtained by introducing an exogenous modifier into the clay material and then uniformly mixing different materials.
The prior disclosed preparation method for synthesizing modified clay by introducing an external flocculating agent generally has the problems of resource waste, high energy consumption, more waste material and waste water discharged from intermediate products and the like; in addition, in the existing preparation process, the synthetic components of the modified clay need to be produced respectively, such as clay powder processing, flocculant preparation and the like, so that the problems of complex overall process, difficult product quality control and low production efficiency exist. How to further improve the algae removal capability of the modified clay, simplify the production flow of the modified clay, reduce the resource occupancy rate, eliminate the pollutant production and discharge, and realize the industrial production of the high-efficiency modified clay material is still the problem that the modified clay method needs to be solved urgently in the process of preventing and controlling the harmful algal blooms.
Disclosure of Invention
Aiming at the problems of the existing preparation method of the modified clay material suitable for preventing and treating the harmful algal blooms, the invention aims to provide a clay modification method suitable for preparing the material for preventing and treating the harmful algal blooms.
In order to achieve the purpose, the invention adopts the technical scheme that:
a clay modifying method for preparing the material to prevent and treat the harmful algal bloom features that the natural clay mineral is used as basic material, which is pulverized into powdered clay, and then temp-controlled calcining → acid activating → secondary neutralization → alkali neutralizing → secondary mixing → temp-controlled ageing is used to compound the basic material to obtain the modified clay with high effect to eliminate the harmful algal bloom.
The reaction can continuously treat the natural clay mineral in a reaction tank, and realizes the modification treatment by a one-tank method to obtain the modified clay. The processing and treatment process of the one-pot method does not generate any toxic and harmful pollutants or wastes.
The reaction can realize the steps of compound treatment of the natural clay minerals in different reaction tanks, and finally the modified clay powder is obtained.
Further, the whole treatment process of the clay modification treatment method is preferably carried out in one reaction vessel, but any operation of increasing the number of reaction tanks or changing the shape of the reactor is also possible to achieve the object of the method of the present invention; the continuous treatment is implemented gradually by the flow type treatment of adding the powdery clay into a reaction tank, controlling the temperature and roasting → adding acid for activation → adding neutralization → adding alkali for neutralization → adding mixing → controlling the temperature and curing, and the like.
The modified clay is dehydrated and crushed to obtain the powder modified clay which is easy to package, transport and store and is suitable for preventing and controlling harmful algal blooms.
Roasting the powder clay at a controlled temperature to obtain roasted clay for later use; carrying out acid activation reaction on part of the calcined clay to obtain activated calcined clay, and then adding the part of the calcined clay which is not activated into a reaction tank for secondary neutralization reaction to obtain primary neutralized clay; adding alkali into the primary neutralized clay to adjust the pH of the system to 3.5-4.5 to obtain alkali neutralized clay; adding powdery clay (pulverized powdery clay is prepared by pulverizing natural clay mineral as base material) into the alkali-neutralized clay, mixing to obtain wool-modified clay, and aging under controlled temperature to obtain wet-modified clay suitable for preventing and treating harmful algal bloom.
Heating and roasting the powder clay at 600-900 ℃ for 0.5-6 h to obtain roasted clay, wherein one part of the roasted clay is left in a reaction tank, one part of the roasted clay is taken out of the reaction tank, and the mass ratio of the roasted clay left in the reaction tank to the roasted clay taken out of the reaction tank is 10 (1-100) for later use;
activating and reacting the part of the calcined clay left in the reaction tank for 1-24 hours at 50-150 ℃ by acid to obtain activated calcined clay, wherein the molar weight of dissociable hydrogen ions in the acid is 2-10 times of the active aluminum content in the calcined clay to be activated;
then filling the taken-out unactivated roasted clay into the reaction tank again, and carrying out a secondary addition neutralization reaction for 1-24 hours at 50-150 ℃ to obtain primary neutralized clay for later use;
controlling the temperature to be 50-85 ℃, adding alkali into the primary neutralized clay, and adjusting the pH of the system to be 3.5-4.5 to obtain alkali neutralized clay; adding powdery clay into the alkali-neutralized clay and uniformly mixing to obtain wool modified clay; wherein the mass ratio of the alkali-neutralized clay to the powdery clay is 1: 0-10;
and curing at the temperature of 50-85 ℃ for 2-24 hours to obtain the wet modified clay suitable for preventing and treating the harmful algal blooms.
In a further aspect of the present invention,
crushing natural clay minerals, heating and roasting at 700 ℃ for 2.5-4 hours to obtain roasted clay, leaving a part of the roasted clay in a reaction tank, taking a part of the roasted clay out of the reaction tank, and controlling the mass ratio of the roasted clay left in the reaction tank to the roasted clay taken out of the reaction tank to be 1: 1-1.5 for standby;
activating and reacting the part of the roasted clay remained in the reaction tank for 2.5-5 hours at 120-130 ℃ by acid to obtain activated roasted clay, wherein the molar quantity of dissociable hydrogen ions in the acid is 3-5 times of the quantity of active aluminum in the roasted clay to be activated;
then filling the taken-out unactivated roasted clay into the reaction tank again, and carrying out a secondary addition neutralization reaction for 2-5 hours at 120-130 ℃ to obtain primary neutralized clay for later use;
controlling the temperature to be 65-70 ℃, adding alkali into the primary neutralized clay, and adjusting the pH value of the system to 3.8-4.2 to obtain alkali neutralized clay; adding powdery clay into the alkali-neutralized clay and uniformly mixing to obtain wool modified clay; wherein the mass ratio of the alkali-neutralized clay powder clay is 1 (1-5);
and curing at 65-70 ℃ for 10-12 h to obtain the wet modified clay suitable for preventing and treating the harmful algal blooms.
The acid in the acid activation is inorganic acid; the acid can be hydrochloric acid, sulfuric acid, phosphoric acid, etc., preferably hydrochloric acid. The alkali compound in the alkali neutralization is a material which can be ionized to generate hydroxide ions; the alkaline compound is selected from sodium carbonate, sodium bicarbonate, sodium hydroxide, potassium hydroxide, ammonia water, etc., preferably sodium carbonate.
The natural clay mineral is clay mineral with aluminosilicate as main chemical componentThe chemical formula of which is usually mAl2O3·nSiO2·zH2O (m, n, z are numbers), and includes minerals such as kaolinite, montmorillonite, illite, chlorite, illite, smectite, attapulgite, sepiolite and the like, and mixed minerals containing two or more thereof, and among them, natural minerals of the kaolinite group having an alumina content of more than 30% are preferable.
The dehydration is to dehydrate the wet modified clay with high water content at the temperature of less than 85 ℃ until the water content is less than 10 percent, preferably less than or equal to 5 percent; the crushing is to process the dried modified clay material into powder with the granularity less than 300 meshes.
The invention has the advantages and positive effects that:
the invention takes natural clay mineral as a base material, obtains the modified clay material with high-efficient elimination capability to harmful algal bloom organisms after a series of composite treatment, and the proposed 'one-pot method' processing technology is suitable for clay mineral materials of different grades, and can prepare a harmful algal bloom organism elimination agent with higher efficiency than the existing method while reducing the production cost; because the green natural clay mineral is adopted as the base material, the excellent chemical composition of the natural clay mineral is fully utilized, and the activity of the natural clay mineral is improved through necessary physical and chemical treatment, so that no toxic and harmful pollutant or waste is generated in the whole treatment process, the processing process or the final product meets the green environmental protection standard, and the efficient comprehensive utilization of mineral resources is realized; the method and the process have good application and popularization values because the different links of the process are clear in hierarchy and continuous in order, thereby facilitating the process control and the realization of batch production during the industrial preparation of the modified clay material.
Drawings
FIG. 1 is a schematic flow chart of a process for preparing modified clay by a one-pot method according to an embodiment of the present invention.
FIG. 2 is a graph comparing the efficiency of removing Prorocentrum donghaiense with different modified clays according to the present invention.
FIG. 3 is a graph comparing the removal efficiency of phaeocystis globosa with different modified clays according to the present invention.
Detailed Description
The present invention will be described in more detail below with reference to examples, but the present invention is not limited thereto, and the method for preparing the modified clay material having high elimination ability against harmful algal bloom organisms will be described in more detail.
The composite treatment of the invention is preferably a one-pot method process, and the treatment is completed in flowing water step by step in one reaction pot. The method is suitable for clay mineral materials of different grades, and can prepare a harmful algal bloom remover which is more efficient than the existing method for synthesizing the modified clay; because the green natural clay mineral is used as the base material, no toxic and harmful pollutant or waste is generated in the treatment process, the processing process and the final product both meet the green environmental protection standard, and the high-efficiency comprehensive utilization of resources can be realized; the different links of the process are continuous and clear, thereby facilitating the process control and batch production of the modified clay material in the industrial preparation.
Example 1
The preparation of the material suitable for preventing and controlling harmful algal blooms by the one-pot method is shown in figure 1:
selecting commercially available powdered kaolin (with the particle size of 500 meshes), weighing 100g of kaolin, adding the kaolin into a stainless steel cylindrical reaction tank, electrically heating to control the temperature, and roasting at 700 ℃ for 2.5 hours; after cooling, the calcined kaolin is divided into two equal parts by weight, one of which is taken out for use.
Adding 200mL of 25 wt% hydrochloric acid into the calcined kaolin remained in the reaction tank at one time, controlling the temperature of the reaction tank to be 130 ℃, and reacting for 4 hours under slow stirring; and adding the other part of the calcined kaolin into the reaction tank after cooling, heating to 130 ℃, continuously stirring for reaction for 2 hours, cooling to 70 ℃, gradually adding sodium carbonate until the pH value is increased to 4.2, maintaining the temperature of the reaction tank at 70 ℃, continuously reacting for 24 hours, adding 100g of commercially available kaolin powder, uniformly mixing, and carrying out curing reaction for 24 hours at 70 ℃ to obtain a modified clay suspension, wherein the modified clay suspension is marked as liquid-I.
The modified clay suspension obtained above can be dried by blowing at 70 deg.C to obtain powdery modified clay material, and is labeled as powder-I.
Example 2
Selecting montmorillonite ore from Weifang city, pulverizing to 200 mesh with ball mill, weighing 100g, adding into stainless steel cylindrical reaction tank, electrically heating to control temperature, and calcining at 600 deg.C for 3 hr; after cooling, dividing the roasted montmorillonite into two parts with the weight ratio of 1:2, and taking out one more part for later use.
Adding 150mL of 20% hydrochloric acid into the calcined montmorillonite left in the reaction tank at one time, controlling the temperature of the reaction tank to be 130 ℃, and reacting for 4 hours under slow stirring; and adding the other part of the calcined montmorillonite into the reaction tank after cooling, heating to 100 ℃, continuing stirring for reaction for 4 hours, cooling to 50 ℃, gradually adding sodium carbonate until the pH value is increased to 4.0, maintaining the temperature of the reaction tank at 50 ℃, and continuing the reaction for 24 hours to obtain a modified clay suspension labeled as liquid-II.
The modified clay suspension obtained above can be dried by blowing at 50 deg.C to obtain powdery modified clay material, labeled as powder-II.
Example 3
Selecting powdery kaolin produced in Guangxi Hepu, weighing 100g of the powdery kaolin, adding the powdery kaolin into a stainless steel cylindrical reaction tank, controlling the temperature by adopting electric heating, and roasting for 2.5 hours at 750 ℃; after cooling, the calcined kaolin is divided into two parts of equal weight for later use, and one part is taken out of the reaction tank.
Adding 250mL of 15% hydrochloric acid into the calcined kaolin remained in the reaction tank at one time, controlling the temperature of the reaction tank to be 130 ℃, and reacting for 3 hours under slow stirring; and adding the other part of the calcined kaolin into the reaction tank after cooling, heating to 130 ℃, continuously stirring for reaction for 3 hours after adding, cooling to 60 ℃, gradually adding sodium carbonate until the pH value is increased to 4.1, maintaining the temperature of the reaction tank at 60 ℃, continuously reacting for 24 hours, adding 50g of commercially available kaolin powder, uniformly mixing, and carrying out curing reaction for 24 hours at 60 ℃ to obtain a modified clay suspension, wherein the modified clay suspension is marked as liquid-III.
The modified clay suspension obtained above can be dried by blowing at 65 deg.C to obtain powdery modified clay material, labeled as powder-III.
Example 4
Selecting commercially available powdered kaolin (500 meshes), weighing 100g of kaolin, respectively adding the kaolin into a stainless steel cylindrical reaction tank A and a stainless steel cylindrical reaction tank B, electrically heating to control the temperature, and roasting at 700 ℃ for 2.5 hours for later use.
Adding 300mL of 25% hydrochloric acid into the calcined kaolin in the reaction tank A at one time, controlling the temperature of the reaction tank at 130 ℃, and reacting for 4 hours under slow stirring; adding the roasted kaolin in the tank B into the reaction tank A after cooling, heating to 130 ℃, continuing stirring for reaction for 2h, cooling to 70 ℃, gradually adding sodium carbonate until the pH value is increased to 4.2, maintaining the temperature of the reaction tank at 70 ℃, continuing the reaction for 24h, adding 100g of commercially available kaolin powder, uniformly mixing, and carrying out aging reaction for 24h at 70 ℃ to obtain a modified clay suspension, wherein the modified clay suspension is marked as liquid-V.
The modified clay suspension obtained above can be dried by blowing at 70 deg.C to obtain powdery modified clay material, and is labeled as powder-V.
Application example
The modified clay suspension obtained in the above example, as well as the PAC modified clay and unmodified clay prepared by the conventional method were used as sample samples, and the algae removal performance of the sample samples was compared with that of the target organisms eliminated by using the common harmful algal blooms in the offshore region of china, proocentrum donghaiense, and proocentrum donghaiense, as the target organisms. The specific experimental method is described in the literature (Qiuhuixia, Shuximing, Caochi Hua, Song Xixianxian, Liu Yang, Zhongyi, 2017. removal of Phaeocystis globosa (Phaeocystis globosa) and prooceanic dinoflagellate (Prorocentrum donghaiense)) by modified clay, ocean and lake marsh, 05: 982-. The final concentration of each clay in the experiment was 0.5g/L, and the results of algae removal in the test are shown in FIGS. 2 and 3. The result shows that the algae removal efficiency of the modified clay material prepared by the embodiment of the invention is obviously higher than that of unmodified clay and PAC modified clay; the modified clay material prepared by adopting a plurality of tanks also has good algae removal capability, but is not more economical and easier to manage than the 'one-tank method' in the invention considering that a plurality of tank process lines in the actual production process need more investment and maintenance. The above description is only an embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, improvement, extension, etc. made within the spirit and principle of the present invention are included in the protection scope of the present invention.
Claims (7)
1. A clay modification method suitable for preparing a harmful algal bloom prevention and control material is characterized by comprising the following steps: the method comprises the following steps of (1) taking natural clay mineral as a base material, crushing the natural clay mineral into powder clay, and then performing temperature-controlled roasting → acid activation → secondary addition neutralization → alkali neutralization → secondary addition mixing → temperature-controlled curing to realize composite treatment on the base material, thereby obtaining the modified clay with high-efficiency elimination capability on harmful algal bloom organisms;
continuously treating natural clay minerals in a reaction tank to realize one-tank modification treatment to obtain modified clay;
specifically, the powder clay is roasted at a controlled temperature to obtain roasted clay for later use; carrying out acid activation reaction on part of the calcined clay to obtain activated calcined clay, and then adding the part of the calcined clay which is not activated into a reaction tank for secondary neutralization reaction to obtain primary neutralized clay; adding alkali into the primary neutralized clay to adjust the pH of the system to 3.5-4.5 to obtain alkali neutralized clay; and adding powdery clay into the alkali-neutralized clay, uniformly mixing to obtain wool product modified clay, and curing at controlled temperature to obtain the wet modified clay suitable for preventing and treating harmful algal bloom.
2. The method for modifying clay suitable for the production of harmful algal bloom controlling material according to claim 1, wherein: the modified clay is dehydrated and crushed to obtain the powder modified clay which is easy to package, transport and store and is suitable for preventing and controlling harmful algal blooms.
3. The method for modifying clay suitable for the production of harmful algal bloom controlling material according to claim 1, wherein:
heating and roasting the powder clay at 600-900 ℃ for 0.5-6 h to obtain roasted clay, wherein one part of the roasted clay is left in a reaction tank, one part of the roasted clay is taken out of the reaction tank, and the mass ratio of the roasted clay left in the reaction tank to the roasted clay taken out of the reaction tank is 10 (1-100) for later use;
activating and reacting the part of the roasted clay remained in the reaction tank for 1-24 hours at 50-150 ℃ by acid to obtain activated roasted clay, wherein the molar weight of dissociable hydrogen ions in the acid is 2-10 times of the active aluminum content in the roasted clay to be activated;
then filling the taken-out unactivated roasted clay into the reaction tank again, and carrying out a secondary addition neutralization reaction for 1-24 hours at 50-150 ℃ to obtain primary neutralized clay for later use;
controlling the temperature to be 50-85 ℃, adding alkali into the primary neutralized clay, and adjusting the pH of the system to be 3.5-4.5 to obtain alkali neutralized clay; adding powdery clay into the alkali-neutralized clay and uniformly mixing to obtain wool modified clay; wherein the mass ratio of the alkali-neutralized clay to the powder clay is 1: 0-10;
and curing at the temperature of 50-85 ℃ for 2-24 hours to obtain the wet modified clay suitable for preventing and treating the harmful algal blooms.
4. The method for modifying clay suitable for the production of harmful algal bloom controlling material according to claim 3, wherein:
crushing the natural clay mineral, heating and roasting at 700 ℃ for 2.5-4 h to obtain roasted clay, leaving a part of the roasted clay in a reaction tank, taking a part of the roasted clay out of the reaction tank, wherein the mass ratio of the roasted clay left in the reaction tank to the roasted clay taken out of the reaction tank is 1: 1-1.5 for standby;
activating and reacting the part of the roasted clay remained in the reaction tank for 2.5-5 hours at 120-130 ℃ by acid to obtain activated roasted clay, wherein the molar quantity of dissociable hydrogen ions in the acid is 3-5 times of the quantity of active aluminum in the roasted clay to be activated;
then filling the taken-out unactivated roasted clay into the reaction tank again, and carrying out a secondary addition neutralization reaction for 2-5 hours at 120-130 ℃ to obtain primary neutralized clay for later use;
controlling the temperature to be 65-70 ℃, adding alkali into the primary neutralized clay, and adjusting the pH value of the system to 3.8-4.2 to obtain alkali neutralized clay; adding powdery clay into the alkali-neutralized clay and uniformly mixing to obtain wool modified clay; wherein the mass ratio of the alkali-neutralized clay powder clay is 1 (1-5);
and curing at 65-70 ℃ for 10-12 h to obtain the wet modified clay suitable for preventing and treating the harmful algal blooms.
5. The method for modifying clay suitable for the production of harmful algal bloom controlling material according to claim 1, wherein: the acid in the acid activation is inorganic acid; the alkali compound in the alkali neutralization is a material that can be ionized to generate hydroxide ions.
6. The method for modifying clay suitable for the production of harmful algal bloom controlling material according to claim 1, wherein: the natural clay mineral is clay mineral containing aluminosilicate as main chemical component, and the main component has chemical formula of mAl2O3·nSiO2·zH2O, including kaolinite, montmorillonite, illite, chlorite, illite-smectite mixed layer, chlorite-smectite mixed layer, attapulgite and sepiolite minerals and mixed minerals containing two or more of them.
7. The method for modifying clay suitable for the production of harmful algal bloom controlling material according to claim 2, wherein: the dehydration is to dehydrate the wet modified clay with high water content at the temperature of less than 85 ℃ until the water content is less than 10 percent; the crushing is to process the dried modified clay material into powder with the granularity less than 300 meshes.
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| AUPO589697A0 (en) * | 1997-03-26 | 1997-04-24 | Commonwealth Scientific And Industrial Research Organisation | Sediment remediation process |
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