CN107235503A - The method that bromo solid waste prepares luminescent material lanthanum oxybromide is decomposed based on mechanical force and chemical - Google Patents
The method that bromo solid waste prepares luminescent material lanthanum oxybromide is decomposed based on mechanical force and chemical Download PDFInfo
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- CN107235503A CN107235503A CN201710307947.0A CN201710307947A CN107235503A CN 107235503 A CN107235503 A CN 107235503A CN 201710307947 A CN201710307947 A CN 201710307947A CN 107235503 A CN107235503 A CN 107235503A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/253—Halides
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7701—Chalogenides
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
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Abstract
Prepared the invention belongs to new material and environmental pollution waste processing arts, it is more particularly to a kind of that the method that bromo solid waste prepares luminescent material lanthanum oxybromide is decomposed based on mechanical force and chemical.This method is at normal temperatures and pressures, it is placed in after bromo solid waste is mixed with reaction reagent in planetary milling reactor, the mechanical force induced chemical reaction produced using ball milling, prepares luminescent material lanthanum oxybromide, and realizes the decomposition of bromo pollutant in the process.The inventive method has advantages below：Technological process is simple, reaction condition is gentle (under normal temperature and pressure), preparation process is without using organic solvent, the product ultimately generated is luminescent material lanthanum oxybromide, and bromo pollutant is thoroughly decomposed in the process, during do not produce secondary pollution, bromo pollutant is added and reacted according to stoichiometric proportion with reaction reagent, meets the theory of Green Chemistry.
Description
Technical field
Prepared the invention belongs to new material and environmental pollution waste processing arts, it is more particularly to a kind of based on machinery
The method that power chemical breakdown bromo solid waste prepares luminescent material lanthanum oxybromide.
Background technology
As a kind of typical rare earth Oxybromide, lanthanum oxybromide (LaOBr) has relatively low phonon energy, in light, electricity, magnetic
In terms of there is unique performance, especially in luminescent material, it is considered to be a kind of good luminous host.Due to LaOBr things
Physicochemical stability is good, nontoxic pollution-free, and it is increasingly becoming the important luminescent material of a class, all has in many fields very wide
Wealthy application prospect, is such as used for laser, quantum counter, X-ray intensifying screen, optical data memories and fluorescence labeling instrument
Deng.
At present, LaOBr preparation method mainly includes sol-gel process, high temperature solid-state method, thermal decomposition method etc., reacts bar
Part is all quite harsh, or needs accurately to control temperature change, or needs carefully to consider solvent, and these sides
Method also has strict requirements to the species and purity of raw material.In recent years, the solvent-free conjunction by representative of mechanochemistry synthesis
Got the attention into (Solvent-Free Synthesis) method, it uses consolidating between mechanical force induction solid material
Phase reaction to be to synthesize target product (i.e. mechanochemistry synthesis), it is to avoid the use of organic solvent, meets the reason of Green Chemistry
Read, be a kind of very method of the synthesis LaOBr with application prospect.
At the same time, as a kind of mode of non-burning, mechanical force and chemical is also applied to halo persistency organic contaminant
Among the decomposition of thing (POPs), i.e., haloginated polluants and reaction reagent generation dehalogenation reaction are induced using mechanical force, reach degraded
Pollutant is simultaneously allowed to innoxious effect (i.e. mechanical force and chemical is decomposed).(such as PBDEs, many bromines for bromo POPs
Biphenyl, many bromobenzenes etc.), its usage amount is huge (other up to ton), at the method only with mechanical force and chemical
Reason will cause the great wasting of resources without being recycled to bromo element.
Therefore, for the angle disposed from Green Chemistry and actual waste, in addition it is also necessary to enterprising in the technique of mechanical force and chemical
The further optimization of row and innovation, mechanochemistry synthesis and mechanical force and chemical are decomposed and combine the synthesis for carrying out LaOBr.
The present invention adds reaction reagent i.e. by the use of bromo solid waste (PBDEs, PBBs, many bromobenzenes etc.) as raw material
La2O3, issue biochemical reaction in the induction of mechanical force, finally can not only synthesizing luminescent material LaOBr, and can reach
The purpose of bromo pollutant is decomposed, is had a great deal of practical meanings.
The content of the invention
In view of the shortcomings of the prior art, decomposing bromo solid waste based on mechanical force and chemical the invention provides one kind prepares hair
The method of luminescent material lanthanum oxybromide.
A kind of to decompose the method that bromo solid waste prepares luminescent material lanthanum oxybromide based on mechanical force and chemical, it utilizes bromine
For organic pollution solid waste as raw material, it is allowed to chemically react under conditions of mechanical force with reaction reagent, synthesizes
Luminescent material lanthanum oxybromide, while realizing the decomposition of bromo pollutant and innoxious, concrete scheme is as follows：In normal temperature and pressure bar
Under part, it is placed in after bromo solid waste is proportionally mixed with reaction reagent in the ball grinder of planetary high-energy ball mill, to
Abrading-ball is added in tank and is sealed, the mechanical force induced chemical reaction produced using ball milling prepares luminescent material lanthanum oxybromide, and
The decomposition of bromo solid pollutant is realized in the process.
Bromo solid waste of the present invention needs to carry out pre-treatment before the reaction, locates before bromo solid waste is carried out
Reason, determines its specific species and bromine content, calculates the time needed for the adding proportion and ball-milling reaction of reaction reagent.
Bromo solid waste of the present invention includes the one or more in PBDEs, PBBs, many bromobenzenes etc..
Reaction reagent of the present invention is La2O3Solid, the addition of itself and bromo solid waste is compared for La:Br=1:1 (rubs
You compare), react generation luminescent material bromine LaOBr completely just.
Ball mill of the present invention is planetary high-energy ball mill.
The rotating speed of ball mill of the present invention is 400~800rpm, preferably 700rpm.
In ball mill running of the present invention 15min is shut down after every continuous service 15min.
The preferred internal diameter of ball grinder of the present invention is 40mm, and dischargeable capacity is 45mL.
Ball radius in ball grinder of the present invention is preferably 15mm, and average weight is 10.5g.
Beneficial effects of the present invention are：
1) using the method for mechanical force and chemical, without harsh reaction condition and control, i.e., can quickly it prepare luminous
Material lanthanum oxybromide.
2) present invention synthesize lanthanum oxybromide while, realize effective decomposition of bromo solid waste, realize product without
Machine and innoxious purpose.
3) present invention is using bromo solid waste as raw material, and it is La with the mol ratio that reaction reagent is added:Br=1:1,
Just reaction generation lanthanum oxybromide completely, not only realizes in waste the recycling of whole bromo elements, also save raw material and
Cost, meets green chemical concept.
4) mechano-chemical reation is solid phase reaction, is not related to organic solvent, is produced without harmful secondary pollution.
5) technological process is simple, and reaction condition is gentle, and operating cost is cheap.
The inventive method W-response technological process is simple, gently (under normal temperature and pressure), energy consumption are relative for reaction condition
It is relatively low, induce bromo solid waste using mechanical force and chemically reacted with reaction reagent, being capable of fast synthesizing luminescent material bromine
Lanthana, and bromo pollutant is thoroughly decomposed in the process and whole bromo elements are utilized, whole process will not have been produced
Evil gas or liquid, meet the theory of Green Chemistry.
Brief description of the drawings
Fig. 1 is the process flow diagram of the inventive method.
Fig. 2 is bromo solid waste and reaction reagent La in embodiment 12O3The X-ray of sample after mixing and ball milling different time
Diffraction (XRD) analysis chart.
Fig. 3 is bromo solid waste and reaction reagent La in embodiment 22O3Pollutant is surplus after mixing and ball milling different time
Remaining situation.
Fig. 4 is bromo solid waste and reaction reagent La in embodiment 32O3The thermogravimetric of sample after mixing and ball milling different time
Analyze (TG/DTA) figure.
Fig. 5 is bromo solid waste and reaction reagent La in embodiment 42O3The Raman of sample after mixing and ball milling different time
Analysis chart.
Embodiment
Below, the accompanying drawing in the embodiment of the present invention will be combined, the technical scheme in the embodiment of the present invention will be carried out in detail
Description, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on this hair
Embodiment in bright, the every other reality that those of ordinary skill in the art are obtained on the premise of creative work is not made
Example is applied, the scope of protection of the invention is belonged to.
It should be noted that herein, term " comprising ", "comprising" or its any other variant are intended to non-row
His property is included, so that process, method, article or equipment including a series of key elements not only include those key elements, and
And also including other key elements being not expressly set out, or also include for this process, method, article or equipment institute inherently
Key element.The invention provides a kind of side that luminescent material lanthanum oxybromide is prepared based on mechanical force and chemical decomposition bromo solid waste
Method, this method is allowed to send out under conditions of mechanical force with reaction reagent by the use of bromo organic pollution solid waste as raw material
Biochemical reaction, synthesizing luminescent material lanthanum oxybromide, while realizing the decomposition of bromo pollutant and innoxious.With reference to attached
The present invention will be further described with embodiment for figure.
Embodiment 1
In order to probe into bromo solid waste and reaction reagent whether to there occurs mechano-chemical reation in mechanical milling process
Lanthanum oxybromide is generated, is tested bromo solid waste and La2O3According to mol ratio La：Br=1:Row is added to after 1 ratio mixing
In planetary high-energy ball milling reactor, control experiment is carried out according to the schematic flow sheet shown in Fig. 1.Ten have been used in this experiment altogether
Dibromodiphenyl ether, decabromodiphenyl, three kinds of bromo solid waste of HBB, have obtained similar result, for convenience of expression, this implementation
Representative is used as using the result of deca-BDE in example.
By 1.888g reaction reagents La2O3(ensure Bi with 1.112g deca-BDEs：Br mol ratio is 1：1) after mixing
Be added in ball grinder (internal diameter 40mm, dischargeable capacity about 45mL), then add into ball grinder 7 abrading-balls (diameter 15mm, it is average
Weight 10.5g) and seal.Ball grinder is fixed on planetary ball mill after the completion of charging, the revolution of ball mill rotating disk is set
Rotating speed is 700rpm, shuts down 15min coolings after every continuous service 15min, after the specific time is run, takes out ball grinder, by
Sample powder carries out XRD analysis after collecting is determined, and resulting result is as shown in Figure 2.
As seen from Figure 2, for La2O3For mixture of the bromo solid waste without ball milling, its XRD diffraction maximum
Mostly come from La2O3Also some irregular little diffraction maximums occur near (in Fig. 2 ● shown), bromo solid waste
(as shown in zero in Fig. 2).After the ball milling by 2h, La2O3Diffraction peak intensity substantially reduce, while in collection of illustrative plates occur
A kind of diffraction maximum of novel substance, understands through XRD database retrievals, and newly-generated material is LaOBr (as shown in the ▼ in Fig. 2)
Crystal.After reaction has carried out 4h, La in sample2O3Diffraction maximum be wholly absent, collection of illustrative plates is by LaOBr diffraction maximum master
Lead, and LaOBr crystal is a kind of luminescent material of good performance, is had a good application prospect.This absolutely proves, mechanical milling process
In there occurs mechano-chemical reation, generate luminescent material LaOBr.
It is also worth noting that La2O3It is remaining without 0 after the completion of reaction as reaction reagent, illustrate itself and bromo
Solid waste according to addition stoichiometric proportion (mol ratio La:Br=1:1) reaction completely, generates LaOBr.
Embodiment 2
In order to confirm the decomposition situation of the bromo solid waste in mechanical milling process, using condition in the same manner as in Example 1
Tested, and remaining target substance in sample is analyzed.When determining, the sample powder after 0.05g ball millings is taken, plus
Enter to 50mL n-hexane and acetone mixed solution in (the wherein volume ratio V/V=1 of n-hexane and acetone:1) it is, ultrasonic
Remaining organic matter in 10min extraction samples, extract solution uses Gas Chromatography-Negative chemical source-mass spectrum (GC-NCI- after processing
MS the content of remaining target substance) is determined, acquired results are as shown in Figure 3.From figure 3, it can be seen that bromo solid waste with
La2O3During mixing and ball milling, with the increase of Ball-milling Time, the concentration of remaining bromo pollutant is gradually reduced in sample,
Its degradation rate has reached 100% after ball milling 4h, and depositing for obvious organic matter has not been observed yet in corresponding GC-MS collection of illustrative plates
Illustrating under conditions of mechanical force, bromo organic matter and La2O3Chemically reacted, not only generate luminescent material
LaOBr, also makes bromo pollutant effectively degrade.
Embodiment 3
In order to further verify the inorganization effect of the bromo solid waste in mechanical milling process, using with phase in embodiment 1
Same condition is tested, and using thermogravimetric (TG/DTA) to sample (0h mixing, 1h ball millings, 2h ball millings and the 4h balls after ball milling
Mill) to be analyzed, resulting result is as shown in Figure 4.
As shown in Figure 4, for bromo solid waste and La2O3Mixture for, with the rise of temperature, sample is 325
~425 DEG C have one close to 37% weight loss, due to La in the mixture2O3Weight will not be produced with the rise of temperature
Change, only the decomposition of bromo organic matter can produce weight loss, therefore this part weightlessness comes from the heat of bromo organic matter
Decompose, ratio of its ratio also with its initial addition matches (the common 3.0g=37.1% of 1.112g/).By 1h's and 2h
After ball milling, be in the weight loss near 325~425 DEG C and persistently reduce, illustrate in mechanical milling process bromo organic matter with
La2O3It there occurs mechanico-chemical reaction and gradually decomposed.For the sample after ball milling 4h, in the temperature in thermogravimetric analysis
Under without weight loss, and sample is also basic in the heating process of continuation keeps constant weight, and this is absolutely proved in sample
In the presence without organic matter, i.e. bromo solid waste with La2O3Mechanico-chemical reaction in thoroughly degraded and inorganic
Change, eliminate the characteristic of pollutant.
Embodiment 4
In order to more preferably show bromo solid waste and La2O3Course of reaction and mechanism in mechanical milling process, using with implementation
Identical condition is tested in example 1, and uses sample (0h mixing, 2h ball of the Raman spectrum (Raman) to ball milling different time
Mill and 4h ball millings) to be analyzed, the result of resulting collection of illustrative plates change is as shown in Figure 5.
As shown in figure 5, for bromo solid waste and La2O3Mixture for, three groups of responses on Raman spectrum are equal
Come from bromo organic molecule (being herein deca-BDE)：In 1520cm-1Nearby there is a very strong absworption peak, be to come from
The stretching vibration of υ (CC) aromatic rings；It is in 1180~1240cm-1The vibration of left and right comes from the υ (C-O-C) in molecule；It is in
690~1090cm-1Absworption peak be derived from the vibrations of C-Br keys.After the ball-milling reaction by 2h, bromo is come from sample
Three absworption peaks of organic molecule substantially weaken, and illustrate that it has occurred that obvious degraded, the structure (phenyl ring of molecular skeleton
And ehter bond) and C-Br keys be destroyed and be broken；And at the same time, occurred in that on Raman collection of illustrative plates and be in 1312cm-1With
1582cm-1Locate obvious peak, the two peaks are respectively from " D bands " vibration (1330-1380cm in DIC sp2 hydridization-1) and " G bands " (1540-1580cm-1) vibration, represent the generation of amorphous carbon and graphitic carbon.After the ball milling by 4h,
Characteristic peak from Raman spectrograms without bromo organic matter, the response of only remaining obvious " D bands " and " G bands ", this is abundant
Illustrate in mechanical milling process, bromo solid waste and La2O3Mechano-chemical reation is there occurs, will while LaOBr is prepared
Bromo pollutant is degradable and inorganization, and the carbon in molecule exists in the form of amorphous carbon carbon and graphitic carbon.
Beneficial effects of the present invention are：1) using the method for mechanical force and chemical, reaction condition and control without harshness, i.e.,
Luminescent material lanthanum oxybromide can quickly be prepared.2) present invention realizes bromo solid and given up while lanthanum oxybromide is synthesized
Effective decomposition of thing, realizes the inorganization and innoxious purpose of product.3) present invention using bromo solid waste as raw material, its with
The mol ratio of reaction reagent addition is La:Br=1:1, reaction generates lanthanum oxybromide completely just, not only realizes complete in waste
The recycling of portion's bromo element, also saves raw material and cost, meets green chemical concept.4) mechano-chemical reation is solid phase
Reaction, is not related to organic solvent, is produced without harmful secondary pollution.5) technological process is simple, and reaction condition is gentle, and operating cost is honest and clean
Valency.
The inventive method W-response technological process is simple, gently (under normal temperature and pressure), energy consumption are relative for reaction condition
It is relatively low, induce bromo solid waste using mechanical force and chemically reacted with reaction reagent, being capable of fast synthesizing luminescent material bromine
Lanthana, and bromo pollutant is thoroughly decomposed in the process and whole bromo elements are utilized, whole process will not have been produced
Evil gas or liquid, meet the theory of Green Chemistry.
Claims (9)
1. a kind of decompose the method that bromo solid waste prepares luminescent material lanthanum oxybromide based on mechanical force and chemical, its feature exists
In comprising the following steps：Using bromo solid waste as raw material, under normal temperature differential pressure, by bromo solid waste and reaction reagent
It is placed in after proportionally mixing in the ball grinder of ball mill, abrading-ball is added into tank and is sealed, by the ball grinder after the completion of charging
It is fixed on ball mill, luminescent material lanthanum oxybromide is prepared in the generation of the mechanical force induced chemical reaction produced using ball milling,
And the decomposition of bromo solid pollutant is completed in the process.
2. a kind of mechanical force and chemical decomposition bromo solid waste that is based on as claimed in claim 1 prepares luminescent material lanthanum oxybromide
Method, it is characterised in that：Described bromo solid waste needs to carry out pre-treatment before the reaction, determines that its specific species and bromine contain
Amount, calculates the time needed for the adding proportion and ball-milling reaction of reaction reagent.
3. a kind of mechanical force and chemical decomposition bromo solid waste that is based on as claimed in claim 1 prepares luminescent material lanthanum oxybromide
Method, it is characterised in that：The bromo solid waste is the organic pollution solid that different number bromines replace, and can be many bromines two
One or more in phenylate, PBBs, many bromobenzenes etc..
4. a kind of mechanical force and chemical decomposition bromo solid waste that is based on as claimed in claim 1 prepares luminescent material lanthanum oxybromide
Method, it is characterised in that：The reaction reagent is La2O3Solid, it is La with the mol ratio that bromo solid waste is added:Br
=1:1.
5. a kind of mechanical force and chemical decomposition bromo solid waste that is based on as claimed in claim 1 prepares luminescent material lanthanum oxybromide
Method, it is characterised in that：The ball mill is planetary high-energy ball mill.
6. a kind of mechanical force and chemical decomposition bromo solid waste that is based on as claimed in claim 1 prepares luminescent material lanthanum oxybromide
Method, it is characterised in that：The revolution rotating speed of the ball mill is 400~800rpm, preferably 700rpm.
7. a kind of mechanical force and chemical decomposition bromo solid waste that is based on as claimed in claim 1 prepares luminescent material lanthanum oxybromide
Method, it is characterised in that：In the ball mill running 15min is shut down after every continuous service 15min.
8. a kind of mechanical force and chemical decomposition bromo solid waste that is based on as claimed in claim 1 prepares luminescent material lanthanum oxybromide
Method, it is characterised in that：Described ball grinder internal diameter is 40mm, and dischargeable capacity is 45mL.
9. one kind as described in any in claim 1~8 is based on mechanical force and chemical and decomposes the luminous material of bromo solid waste preparation
Expect the method for lanthanum oxybromide, it is characterised in that：Described method is used to prepare luminescent material lanthanum oxybromide and decompose bromo to consolidate
Body waste.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103386314A (en) * | 2013-07-29 | 2013-11-13 | 清华大学 | Method for preparing photocatalyst with visible light response by mechanochemical treatment on polybrominated diphenyl ether solid waste |
| CN106865595A (en) * | 2017-03-06 | 2017-06-20 | 清华大学 | A kind of method that utilization exhausted perfluoro or multi-fluorinated compounds prepare nanometer fluorine lanthana |
-
2017
- 2017-05-04 CN CN201710307947.0A patent/CN107235503A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103386314A (en) * | 2013-07-29 | 2013-11-13 | 清华大学 | Method for preparing photocatalyst with visible light response by mechanochemical treatment on polybrominated diphenyl ether solid waste |
| CN106865595A (en) * | 2017-03-06 | 2017-06-20 | 清华大学 | A kind of method that utilization exhausted perfluoro or multi-fluorinated compounds prepare nanometer fluorine lanthana |
Non-Patent Citations (1)
| Title |
|---|
| GIOVANNI CAGNETTA，ET AL.: "Mechanochemical conversion of brominated POPs into useful oxybromides: a greener approach", 《SCIENTIFIC REPORTS》 * |
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