CN100548516C - The removal method of tetrabromo diphenol A of toxic harmful environ mental pollutant - Google Patents
The removal method of tetrabromo diphenol A of toxic harmful environ mental pollutant Download PDFInfo
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- CN100548516C CN100548516C CNB2005101110635A CN200510111063A CN100548516C CN 100548516 C CN100548516 C CN 100548516C CN B2005101110635 A CNB2005101110635 A CN B2005101110635A CN 200510111063 A CN200510111063 A CN 200510111063A CN 100548516 C CN100548516 C CN 100548516C
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Abstract
The invention belongs to the environment remediation technical field, be specially the removal method of tetrabromo diphenol A of toxic harmful environ mental pollutant.This method is to stir and heating under 90 ℃, aqueous alkali directly is being added drop-wise to a tetrabromobisphenol A, in the Ni-Al alloy and the aqueous solution.Because Ni-Al alloy and aqueous alkali reaction generate hydrogen.The hydrogen reducing that tetrabromobisphenol A is generated in the system generates the debrominate compound bisphenol-A.Bisphenol-A itself is an important chemical material, can be reused.Simultaneously, act as a fuel, also can not produced any poisonous murder gas and other products, only produce carbon dioxide and water by completing combustion.This method technology is simple, and is easy to operate, is easy to large-scale industrial production.The present invention removes the poisonous and harmful tetrabromobisphenol A and becomes useful important industrial chemicals, turns waste into wealth.The natural environment of both having protected us to depend on for existence has been realized the regeneration of natural resources again, is a kind of Green Chemistry method.
Description
Technical field
The invention belongs to the environment remediation technical field, be specially the removal method of tetrabromo diphenol A of toxic harmful environ mental pollutant.
Background of invention
The problem of environmental pollution of persistence toxic chemical substance is the same with depletion of the ozone layer and greenhouse effects and be called 21 century and influence human survival and three healthy overall situation problems.No matter be the 12 class persistence organic pollutants of determining in the Convention of Stockholm, or 12 definite biological accumulation of class persistence and toxic chemical substances of U.S. EPA, and the research of environment incretion interferent is all relevant with the persistence toxic chemical pollutant.After tetrabromo diphenol A of toxic harmful environ mental pollutant is absorbed by the body, cause the mankind spermatozoon vigor to descend, the female ovum mutation, consequently human reproduction's ability drop directly has influence on human reproduction procreation and existence in the future.Therefore, developed country progressively eliminates this product, and develops other substitutes.Be mainly used in plastics as the fire retardant tetrabromobisphenol A, rubber is in the macromolecular materials such as phenolic resin (for example home-use tableware).In recent years, relevant studies have shown that is by using the home-use tableware of phenolic resin, human hyperabsorption tetrabromobisphenol A.After consequently tetrabromobisphenol A is absorbed by the body, cause the mankind spermatozoon vigor to descend, the female ovum mutation, consequently human reproduction's ability drop directly has influence on human existence.Because the tetrabromobisphenol A chemical property is stable, be difficult for handling.Commonsense method uses incinerator to carry out high temperature incineration, and tetrabromobisphenol A not only can not burnedly decompose, and can produce hypertoxic dioxin-like compound on the contrary.The caused pollution problem of tetrabromobisphenol A has caused showing great attention to of international environmental protection tissue, national governments and the common people.The removal Processing Technology Research that tetrabromobisphenol A all is badly in need of carrying out in the world and China is sought economy and practical approach and is handled this type of persistence poisonous and harmful environmental contaminants as early as possible, realizes the reparation of natural environments such as soil and water.Therefore, the removal processing method of studying it is day by day urgent, is to go.
So far, main methods is:
(1) R.Dumler (Chemosphere, 1989,19,2023); J.Thies (Chemosphere, 1990,20,1921); R.Luijk (Chemosphere, 1992,25,361); M.Riess (Chemosphere, 2000,40,937); H.Wichmann people such as (Chemosphere, 2002,47,349) has reported the method for high temperature incineration tetrabromobisphenol A.
(2) people (Ind.Eng.Chem.Res., 2004,43,1952) such as F.Barontini has reported the method that elevated temperature heat is decomposed tetrabromobisphenol A.
Because the tetrabromobisphenol A chemical property is highly stable, during high temperature incineration, not only can not burnedly decompose, can produce hypertoxic dioxin-like compound on the contrary, so there is deadly defect in people's such as Dumler method.People's such as Barontini method is decomposed tetrabromobisphenol A at high temperature (650 ℃), needs high temperature and debrominate fully, does not reach complete debrominate and removes purpose, does not have any use value.
Summary of the invention
It is simple to the objective of the invention is to propose a kind of technology, is easy to form the removal method of the poisonous and harmful tetrabromobisphenol A of scale.
The removal method of the tetrabromobisphenol A that the present invention proposes, its step is as follows: under stirring and heating, aqueous alkali directly is added drop-wise to tetrabromobisphenol A, in the mixed solution of Ni-Al alloy and water.Ni-Al alloy use amount is 1.0-50.0 times (weight ratio) of tetrabromobisphenol A; The control reaction temperature is 20 ℃ ~ 100 ℃.After dropwising, continue to stir 3-6 hour.
Among the present invention, employed aqueous alkali is a NaOH, potassium hydroxide, calcium hydroxide, lithium hydroxide, cesium hydroxide, one or more of baryta water etc.
In the said method, the aqueous alkali concentration of dropping generally can be 0.2-20wt%, and dripping quantity is the 40-150% of aforementioned mixed liquor volume, and the dropping time is 30-80 minute.
Among the present invention, stirring reaction is cooled to room temperature after finishing, and filters, and removes insoluble matter, aqueous solution ethyl acetate extraction, and the organic layer anhydrous magnesium sulfate drying, decompression concentrates.Product after concentrating with high pressure liquid chromatographic analysis, it consists of bisphenol-A, and former tetrabromobisphenol A is transformed fully.
Among the present invention, by Ni-Al alloy and alkali reaction, generate hydrogen, the hydrogen reducing that tetrabromobisphenol A is generated generates nontoxic bisphenol-A.The present invention removes the poisonous and harmful tetrabromobisphenol A and becomes useful important industrial chemicals bisphenol-A, turns waste into wealth.The natural environment of both having protected us to depend on for existence has been realized the regeneration of natural resources again, is a kind of Green Chemistry method.
The inventive method technology is simple, is easy to form large-scale production, is with a wide range of applications.
Concrete experiment method
In the three-necked bottle of embodiment 1:500 milliliter, thermometer is installed, agitator adds tetrabromobisphenol A (10 mMs, 624 milligrams), Ni-Al alloy (10g), and water (100 milliliters) begins to be heated with stirring to 90 ℃ then.With 1 hour dropping 1% sodium hydrate aqueous solution (100 milliliters).The control reaction temperature is 90 ℃-100 ℃.1% sodium hydrate aqueous solution stirred under this temperature 5 hours after dripping and finishing again.Be cooled to room temperature then, filter, elimination insoluble matter, aqueous solution ethyl acetate extraction, organic layer with anhydrous magnesium sulfate drying after, decompression is concentrated.Product after concentrating with the analysis of high pressure liquid phase look general then, the conversion ratio of tetrabromobisphenol A is 100%.
In the three-necked bottle of embodiment 2:500 milliliter, thermometer is installed, agitator, tetrabromobisphenol A (10 mMs, 624 milligrams), Ni-Al alloy (10g), water (120 milliliters) begins to be heated with stirring to 90 ℃ then.With 1 hour dropping 1% potassium hydroxide aqueous solution (120 milliliters).The control reaction temperature is 90 ℃-100 ℃.1% potassium hydroxide aqueous solution stirred under this temperature 6 hours after dripping and finishing again.Be cooled to room temperature then, filter, elimination insoluble matter, aqueous solution ethyl acetate extraction, organic layer with anhydrous magnesium sulfate drying after, decompression is concentrated.Product after concentrating with the analysis of high pressure liquid phase look general then, the conversion ratio of tetrabromobisphenol A is 100%.
In the three-necked bottle of embodiment 3:500 milliliter, thermometer is installed, agitator adds tetrabromobisphenol A (10 mMs, 624 milligrams), Ni-Al alloy (10g), and water (140 milliliters) begins to be heated with stirring to 90 ℃ then.With 1 hour dropping 1% calcium hydroxide aqueous solution (140 milliliters).The control reaction temperature is 90 ℃-100 ℃.1% calcium hydroxide aqueous solution stirred under this temperature 6 hours after dripping and finishing again.Be cooled to room temperature then, filter, elimination insoluble matter, aqueous solution ethyl acetate extraction, organic layer with anhydrous magnesium sulfate drying after, decompression is concentrated.Product after concentrating with the analysis of high pressure liquid phase look general then, the conversion ratio of tetrabromobisphenol A is 100%.
In the three-necked bottle of embodiment 4:500 milliliter, thermometer is installed, agitator adds tetrabromobisphenol A (10 mMs, 624 milligrams), Ni-Al alloy (5g), and water (130 milliliters) begins to be heated with stirring to 90 ℃ then.With 1 hour dropping 0.2% sodium hydrate aqueous solution (130 milliliters).The control reaction temperature is 90 ℃-70 ℃.1% potassium hydroxide aqueous solution stirred under this temperature 6 hours after dripping and finishing again.Be cooled to room temperature then, filter, elimination insoluble matter, aqueous solution ethyl acetate extraction, organic layer with anhydrous magnesium sulfate drying after, decompression is concentrated.Product after concentrating with the analysis of high pressure liquid phase look general then, the conversion ratio of tetrabromobisphenol A is 100%.
Claims (3)
1, a kind of removal method of tetrabromo diphenol A of toxic harmful environ mental pollutant is characterized by: under stirring and heating, aqueous alkali directly is added drop-wise to tetrabromobisphenol A, in the mixed solution of Ni-Al alloy and water; Ni-Al alloy use amount is 1.0-50.0 a times of tetrabromobisphenol A weight, and the control reaction temperature is 20 ℃ ~ 100 ℃; After dripping end, continue to stir 3-6 hour.
2, method according to claim 1 is characterized in that employed aqueous alkali is one or more in NaOH, potassium hydroxide, calcium hydroxide, lithium hydroxide, cesium hydroxide, the baryta water.
3, method according to claim 1, it is characterized in that the aqueous alkali concentration that drips is 0.2-20wt%, dripping quantity is the 40-150% of described mixed liquor volume, the dropping time is after 30-80 minute stirring reaction finishes, to be cooled to room temperature, filters, remove insoluble matter, aqueous solution ethyl acetate extraction, the organic layer anhydrous magnesium sulfate drying, decompression concentrates.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101110635A CN100548516C (en) | 2005-12-01 | 2005-12-01 | The removal method of tetrabromo diphenol A of toxic harmful environ mental pollutant |
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| CNB2005101110635A CN100548516C (en) | 2005-12-01 | 2005-12-01 | The removal method of tetrabromo diphenol A of toxic harmful environ mental pollutant |
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| Publication Number | Publication Date |
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| CN1792478A CN1792478A (en) | 2006-06-28 |
| CN100548516C true CN100548516C (en) | 2009-10-14 |
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| CN102503050B (en) * | 2011-12-20 | 2013-04-03 | 清华大学 | Artificial composite soil layer treatment system capable of reinforcing removal of endocrine disruptors |
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Non-Patent Citations (7)
| Title |
|---|
| anaerobic biotransformation of tetrabromobisphenola,tetrabromobisphenol a,and bisphenol a in estuarinesediments. JAMES W.VOORDECKERS et al.Environ. Sci. Technol.,Vol.36 No.4. 2002 |
| anaerobic biotransformation of tetrabromobisphenola,tetrabromobisphenol a,and bisphenol a in estuarinesediments. JAMES W.VOORDECKERS et al.Environ. Sci.Technol.,Vol.36 No.4. 2002 * |
| anaerobic-aerobic process for microbial degradationoftetrabromobisphenol A. ZEEV RONEN et al.applied and environmental microbiology,Vol.66 No.6. 2000 |
| anaerobic-aerobic process for microbial degradationoftetrabromobisphenol A. ZEEV RONEN et al.applied and environmental microbiology,Vol.66 No.6. 2000 * |
| debromination of duroplastic flame-retarded polymers. Katrin Mackenzie et al.chemosphere,Vol.33 No.12. 1996 |
| debromination of duroplastic flame-retarded polymers. Katrin Mackenzie et al.chemosphere,Vol.33 No.12. 1996 * |
| salt marsh rhizosphere affects microbial biotransformationofthewidespreadhalogenatedcontaminanttetrabromobisphenol-A(TBBPA). B.Ravit et al.soil biology & biochemistry,Vol.37 . 2005 |
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