CN1446749A - Method of microwave synthesizing organic bentonite - Google Patents
Method of microwave synthesizing organic bentonite Download PDFInfo
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- CN1446749A CN1446749A CN 03116258 CN03116258A CN1446749A CN 1446749 A CN1446749 A CN 1446749A CN 03116258 CN03116258 CN 03116258 CN 03116258 A CN03116258 A CN 03116258A CN 1446749 A CN1446749 A CN 1446749A
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Abstract
A process for synthesizing organic bentone by microwave method includes proportionally dissolving the surfactant in water, adding dried and sieved raw bentone, microwave reaction under 100-500 W of power for 10 S-30 min, filter, washing to remove free surfactant, microwave drying at 60-120 deg.C for 0.5-24 hrs, grinding and sieving. Its advantages are short time, low energy consumption, no generation of sewage, and high quality of product.
Description
Technical field
The present invention relates to the synthetic bentonite method of a kind of microwave.More particularly, with the wilkinite original soil or through the wilkinite of acidifying, sodium with after surfactant soln mixes, handle by microwave exposure, ion-exchange takes place, obtain organobentonite.
Background technology
Wilkinite is widely used in industries such as chemical industry, food, oil, agricultural chemicals and environmental protection owing to have fabulous absorption property and ion-exchange performance.In decades, people improve bentonitic characteristic from increasing aspects such as specific surface area, raising saturated extent of adsorption and enlargement layer spacing always, and method commonly used is for using the organic modifiers modified alta-mud.Because correctly handled the interaction relationship of technology and exploitation, the commercial exploitation of organobentonite synthetic technology has obtained very ten-strike.Operational path simplification, investment and process cost descend, environmental friendliness.At present, in order to satisfy special application need, the further expansion of the performance that realizes organising, people are developed to new organobentonite synthesis route direction gradually.But the synthetic cost of bentonite is higher, and when being used for the environment protection aspect, the organic pollutant removal rate is not really high, is directly to influence the reason that wilkinite is used.
Organobentonite is with the interlayer exchangeable cation in organic cation (organic ammonium salt, quaternary ammonium salt etc.) the replacement montmorillonite (bentonitic main component), thereby makes wilkinite be changed into the organobentonite of lipophilic-hydrophobic property by hydrophilic oleophobic property.At present, the synthetic general preparation technology of bentonite mainly contains three kinds.A kind of is dry method, its synthetic method is that the selected sodium bentonite with moisture 20%-30% directly mixes with organic insulating covering agent, homogeneous heating, through being crushed to the organobentonite that contains certain moisture, further drying, be broken into powder-like product or directly be scattered in formation gel or emulsoid product in the organic solvent.This method only reaches the purpose that organises by extruding when modification, facility investment is big, and can't guarantee the homogeneity of product, in addition, this method need be used selected sodium bentonite, and is higher to ingredient requirement, and the most of bentonite ore of China is a calcium base soil, therefore is unfavorable for applying at home.Another kind is the pre-gelled method, and its synthetic method is after wilkinite is separated, retrofits, purifies, to add hydrophobic organic solvent (as mineral oil) in organic overwrite procedure.Hydrophobic wilkinite mixture extraction is entered organic phase, and water phase separated is removed residual moisture through evaporation again and is directly made organobentonite pre-gelled product.Equally, this kind method can not obtain mixing the organobentonite product of homogeneous, and complicated process of preparation, and the products obtained therefrom cost is higher.The third method is that wet method prepares organobentonite, is about to bentonite in powder and is scattered in slurrying in the organically-modified agent solution, retrofits, and then after filtration, oven dry, pulverize, obtains the organobentonite product.This method is to use more Bentonite Modification Technologies at present.But this kind method needs 80 ℃ of left and right sides waters bath with thermostatic control, stirs more than the 2hr when slurrying, time consumption and energy consumption, and have the waste water that contains tensio-active agent in a large number to produce, need further to handle, make this kind method for organic modification very uneconomical, and easily cause the pollution of tensio-active agent.
Summary of the invention
The purpose of this invention is to provide the synthetic bentonite method of a kind of microwave.
It is that tensio-active agent is soluble in water by the 20-200%CEC of the cation exchange capacity of wilkinite original soil, its quality solid-to-liquid ratio scope is 1: 5-1: 500, and the wilkinite original soil that add drying, sieves is put into the microwave reactor of 100-5000W microwave power, irradiation 10s-30min, filter flush away free tensio-active agent, microwave drying, in 60-120 ℃ of oven dry down, drying time is 30min-24hr, grinds, sieves, and obtains organobentonite.
Advantage of the present invention is:
1) the synthetic organobentonite of microwave can shorten the synthetic treatment time greatly.The use microwave exposure is handled, and carries out the wilkinite organic modification, and speed is fast, has shortened the synthetic treatment time, compares with conventional method, in the time of can saving more than 50%.
2) synthesis technique is simplified, and energy consumption significantly reduces.Microwave process for synthesizing can save technologies such as water bath with thermostatic control, stirring, has simplified synthesis technique greatly, saves the water bath with thermostatic control energy saving technology and reaches about 40%.
3) filtrate cycle utilization does not produce the sewage that contains tensio-active agent.
4) the organobentonite constant product quality of Huo Deing, outward appearance homogeneous, cost are lower, good adsorption performance, and it is effective to remove organic pollutant, economical and efficient.
5) be particularly suitable for adopting cationic surfactant that sodium base, calcium-base bentonite or acidic white earth are carried out organic modification.
Embodiment
The synthetic bentonite method of microwave be with wilkinite with after surfactant soln mixes, the use microwave exposure carries out organic modification in the resonant cavity type microwave reactor.Wherein, microwave power, irradiation time, dosage of surfactant etc. have certain change with different original soil kinds.
Consider the absorption problem of micro-wave energy, the preferred wet-process modified process of wilkinite organic modification process.The wilkinite original soil of preferred especially drying and screening carries out radiation modification after mixing with organically-modified agent solution.The wilkinite original soil can be calcium base soil, a sodium base soil or through the acidifying acidic white earth.Organic modifiers can be that (the alkyl carbon number is more than 12 for the long chain type cats product, as CETRIMIDE POWDER), short chain type cats product (the alkyl carbon number is below 10, as tetramethylammonium bromide) and aniorfic surfactant (as sodium lauryl sulphate).Reactor can be selected the rectangular cavity ripple reactor that declines for use.Radiation treatment can adopt batch operation.But the present invention is not limited to this.
The present invention utilizes microwave exposure to carry out the wilkinite wet method and organises, and the wilkinite original soil is to carry out ion-exchange with organic modifiers in the aqueous solution, reaches the purpose of modification.To be higher than the wilkinite original soil because water absorbs the ability of microwave, in microwave field, heat up rapidly, reach boiling very soon.Therefore, the flow arrangement of this technology controlling and process microwave irradiation time evaporates in a large number to avoid the water in the organically-modified agent solution.Keep certain modification temperature, take the pulsed irradiance method to reach, promptly behind the microwave exposure certain hour, stop for some time, treating that water temperature is reduced to carries out irradiation again below the boiling point.
The present invention changes the bentonitic characteristic that organises by the microwave energy of control irradiation.The control of microwave energy is finished by regulating microwave power and irradiation time.For example, when the higher microwave energy of needs, fixedly irradiation time improves the power that microwave source provides; Perhaps constant power, prolongation irradiation time also can increase power simultaneously, prolong irradiation time.Microwave power source magnetron oscillation frequency commonly used is 2450MHz, output rating 100-5000W.Consider the problem of technology time consumption and energy consumption, general irradiation time is 10s-30min.Microwave energy scope of the present invention is not limited to above level.
The present invention regulates bentonitic organic degree by changing the consumption of organic modifiers (being generally tensio-active agents such as ammonium salt, quaternary ammonium salt).The yardstick of dosage of surfactant is the cation exchange capacity (CEC) of wilkinite original soil, and when using single tensio-active agent, consumption is expressed as a certain proportion of CEC.Refer to promptly that as 100%CEC used tensio-active agent quality is suitable with original soil CEC value, products obtained therefrom is cationic organobentonite.When using complexed surfactant, ratio with different proportioning tensio-active agents and CEC value is represented, carry out organic modification as the cationic surfactant of compound use 80%CEC value and the aniorfic surfactant of 20%CEC value, products obtained therefrom is a male-female ionic organobentonite.Organic modifiers consumption of the present invention changes the above level that is not limited to.
Microwave power of the present invention, irradiation time, dosage of surfactant can be chosen wantonly wherein, and one or more change collaborative carrying out.According to the present invention, can in the resonant cavity type microwave reactor, synthesize have lipophilic-hydrophobic property preferably, organobentonite that adsorptive power is bigger.
Must be pointed out that above-mentioned organobentonite kind is cationic, dication type or male-female ionic.But the present invention is not limited to these kinds.According to the characteristic requirement of pending pollutent to the wilkinite performance demands and when being used for environmental protection industry, organobentonite can also comprise many other forms, for example, and anionic, the pillared type of organic-inorganic and other type.
Further specify the present invention below by example, but invention is not limited thereto.
Embodiment 1
Select the calcium-base bentonite in ore deposit, ground after the purification for use, in rectangular cavity declines the ripple reactor, carry out organic modification.Organic modifiers is chloro-hexadecane yl pyridines (CPC), and consumption is 100%CEC, is mixed with surfactant soln at 1: 15 by wilkinite and modifier solution solid-liquid mass ratio, the wilkinite original soil is scattered in the solution microwave power 700W, irradiation 30s-2min.Filter, wash, microwave drying 1-2.5min, 70 ℃ of baking 3hr ground 100 mesh sieves.The organobentonite proterties of gained is stable, and the quality homogeneous is used for the acid blue dye waste water decoloring and handles, and organobentonite is 1: 3000 o'clock with the wastewater quality ratio, is that the decolorization rate of wastewater of 25mg/L can reach more than 95% to dye strength.
Embodiment 2
Select the calcium-base bentonite of Linan industry acidifying remodeling for use, in rectangular cavity declines the ripple reactor, carry out organic modification.Organic modifiers is chloro-hexadecane yl pyridines (CPC) and tetramethylammonium bromide (TMAB), and consumption is CPC: 60%CEC, TMAB: 40%CEC.Press wilkinite and modifier solution solid-liquid mass ratio preparation in 1: 10 surfactant soln, the wilkinite original soil is scattered in the solution microwave power 700W, irradiation time 4min.Filter, wash, microwave drying 1-3min, 80 ℃ of baking 2hr ground 100 mesh sieves.The organobentonite of gained is the pulverulent solids of white loose, is used for the acidic bright red paint waste water decoloring and handles, and organobentonite is 1: 1000 o'clock with the wastewater quality ratio, is that the decolorization rate of wastewater of 25mg/L can reach 99% to dye strength.
Embodiment 3
Select the Inner Mongol calcium-base bentonite for use, behind drying, mistake 100 mesh sieves, in rectangular cavity declines the ripple reactor, carry out organic modification.Organic modifiers is chloro-hexadecane yl pyridines (CPC) and tetramethylammonium bromide (TMAB), and consumption is CPC: 60%CEC, TMAB: 40%CEC.Be mixed with surfactant soln at 1: 12 by wilkinite and modifier solution solid-liquid mass ratio, the wilkinite original soil is scattered in the solution, microwave power 700W, irradiation 1-4min.Filter, wash, microwave drying 1-3.5min, 80 ℃ of baking 3hr ground 100 mesh sieves.The organobentonite proterties of gained is stable, and the quality homogeneous is used for the acid yellow dye waste water decoloring and handles, and organobentonite is 1: 500 o'clock with the wastewater quality ratio, is that the decolorization rate of wastewater of 25mg/L can reach more than 90% to dye strength.
Embodiment 4
Select the calcium-base bentonite in ore deposit, ground after the purification for use, in rectangular cavity declines the ripple reactor, carry out organic modification.Organic modifiers is chloro-hexadecane yl pyridines (CPC) and sodium lauryl sulphate (SDS), and consumption is CPC: 80%CEC, SDS: 20%CEC.Be mixed with surfactant soln at 1: 15 by wilkinite and modifier solution solid-liquid mass ratio, the wilkinite original soil is scattered in the solution, microwave power 1000W, irradiation 1-3min.Filter, wash, microwave drying 2.5min, 70 ℃ of baking 3hr ground 100 mesh sieves.The organobentonite of gained is a lipophilic-hydrophobic property white powder solid, is used to handle p-NP waste water, and organobentonite is 1: 1000 o'clock with the wastewater quality ratio, and concentration is that the waste water p-NP clearance of 50mg/L can reach more than 60%.
Claims (9)
1. a microwave synthesizes the bentonite method, it is characterized in that tensio-active agent soluble in water by the 20-200%CEC of the cation exchange capacity (CEC) of wilkinite original soil, its quality solid-liquid than scope 1: 5-1: 500, the wilkinite original soil that add drying, sieves, put into the microwave reactor of 100-5000W microwave power, irradiation 10s-30min, filter, flush away free tensio-active agent, microwave drying, in 60-120 ℃ of oven dry down, drying time is 30min-24hr, grind, sieve, obtain organobentonite.
2. a kind of microwave according to claim 1 synthesizes the bentonite method, it is characterized in that said range of microwave power at 100-2000W, and the irradiation time scope is at 10s-20min.
3. a kind of microwave according to claim 1 synthesizes the bentonite method, it is characterized in that the cation exchange capacity of said dosage of surfactant scope at the 30%-150% original soil.
4. a kind of microwave according to claim 1 synthesizes the bentonite method, the solid-liquid that it is characterized in that said wilkinite original soil and surfactant soln than scope 1: 5-1: 300.
5. a kind of microwave according to claim 1 synthesizes the bentonite method, it is characterized in that said organobentonite earlier through microwave drying, and be 30s-10min time of drying, and in 60-120 ℃ of oven dry down, drying time is 30min-5hr then.
6. a kind of microwave according to claim 1 synthesizes the bentonite method, it is characterized in that the bentonite origin grogs degree scope that obtains is the 40-200 order.
7. a kind of microwave according to claim 1 synthesizes the bentonite method, it is characterized in that said wilkinite original soil be calcium-base bentonite original soil, sodium bentonite original soil, through the wilkinite of sodium modification, through the acidifying acidic white earth.
8. a kind of microwave according to claim 1 synthesizes the bentonite method, it is characterized in that said kinds of surfactants be the alkyl carbon number at the long chain type cats product more than 12, alkyl carbon number at short chain type cats product and aniorfic surfactant below 10.
9. a kind of microwave according to claim 1 synthesizes the bentonite method, it is characterized in that said microwave reactor adopts the rectangular cavity ripple reactor that declines.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295295A (en) * | 2011-06-13 | 2011-12-28 | 中国石油化工股份有限公司 | Method for preparing organoclay by using composite organic modifier |
| CN102745769A (en) * | 2012-08-02 | 2012-10-24 | 常州大学 | Microwave assisted integrated process for synthesizing and treating oily wastewater by using organic bentonite |
| CN104069822A (en) * | 2014-07-28 | 2014-10-01 | 武汉科技大学 | Microwave organic modified particle bentonite/attapulgite adsorbent and preparation method thereof |
| CN104399222A (en) * | 2014-12-02 | 2015-03-11 | 爱土工程环境科技有限公司 | Composite biomass charcoal waste incineration fly ash treatment stabilizer and preparation method thereof |
| CN105170078A (en) * | 2015-10-08 | 2015-12-23 | 江苏绿田环保科技有限公司 | Preparation method of remediation agent for low-concentration single-type organic pollution |
| CN105921138A (en) * | 2016-06-27 | 2016-09-07 | 东南大学 | Preparation method of modified kaolin for adsorbing semivolatile heavy metals |
| CN112533314A (en) * | 2020-12-01 | 2021-03-19 | 合肥工业大学 | Method for modifying expansive soil by microwave heating |
| CN112694094A (en) * | 2021-03-02 | 2021-04-23 | 辽宁石油化工大学 | Method for preparing sodium bentonite by using sodium fluoride through semidry method under assistance of microwaves |
| CN115583720A (en) * | 2022-09-28 | 2023-01-10 | 江西盖亚环保科技有限公司 | Filler for enhancing biocompatibility and manufacturing method and application thereof |
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2003
- 2003-04-07 CN CN 03116258 patent/CN1210205C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295295A (en) * | 2011-06-13 | 2011-12-28 | 中国石油化工股份有限公司 | Method for preparing organoclay by using composite organic modifier |
| CN102745769A (en) * | 2012-08-02 | 2012-10-24 | 常州大学 | Microwave assisted integrated process for synthesizing and treating oily wastewater by using organic bentonite |
| CN104069822A (en) * | 2014-07-28 | 2014-10-01 | 武汉科技大学 | Microwave organic modified particle bentonite/attapulgite adsorbent and preparation method thereof |
| CN104399222A (en) * | 2014-12-02 | 2015-03-11 | 爱土工程环境科技有限公司 | Composite biomass charcoal waste incineration fly ash treatment stabilizer and preparation method thereof |
| CN104399222B (en) * | 2014-12-02 | 2018-01-23 | 爱土工程环境科技有限公司 | Composite biomass charcoal domestic garbage incineration flyash processing stabilizer and preparation method thereof |
| CN105170078A (en) * | 2015-10-08 | 2015-12-23 | 江苏绿田环保科技有限公司 | Preparation method of remediation agent for low-concentration single-type organic pollution |
| CN105921138A (en) * | 2016-06-27 | 2016-09-07 | 东南大学 | Preparation method of modified kaolin for adsorbing semivolatile heavy metals |
| CN112533314A (en) * | 2020-12-01 | 2021-03-19 | 合肥工业大学 | Method for modifying expansive soil by microwave heating |
| CN112694094A (en) * | 2021-03-02 | 2021-04-23 | 辽宁石油化工大学 | Method for preparing sodium bentonite by using sodium fluoride through semidry method under assistance of microwaves |
| CN112694094B (en) * | 2021-03-02 | 2022-08-09 | 辽宁石油化工大学 | Method for preparing sodium bentonite by using sodium fluoride through semidry method under assistance of microwaves |
| CN115583720A (en) * | 2022-09-28 | 2023-01-10 | 江西盖亚环保科技有限公司 | Filler for enhancing biocompatibility and manufacturing method and application thereof |
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