CN106008595B - A kind of method and device quickly recycling triphenyl phosphate from discarded circuit board - Google Patents
A kind of method and device quickly recycling triphenyl phosphate from discarded circuit board Download PDFInfo
- Publication number
- CN106008595B CN106008595B CN201610391938.XA CN201610391938A CN106008595B CN 106008595 B CN106008595 B CN 106008595B CN 201610391938 A CN201610391938 A CN 201610391938A CN 106008595 B CN106008595 B CN 106008595B
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- Prior art keywords
- circuit board
- isopropanol
- heat treatment
- triphenyl phosphate
- solvent heat
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000004064 recycling Methods 0.000 title claims abstract description 18
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 92
- 239000002904 solvent Substances 0.000 claims abstract description 45
- 238000010438 heat treatment Methods 0.000 claims abstract description 30
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 30
- 239000010935 stainless steel Substances 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000003063 flame retardant Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 9
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 230000035484 reaction time Effects 0.000 abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- 239000000047 product Substances 0.000 description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N n-propyl alcohol Natural products CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 6
- 238000002390 rotary evaporation Methods 0.000 description 5
- 239000012265 solid product Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 229940044613 1-propanol Drugs 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 239000012453 solvate Substances 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical class N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- NDERRIHSWCOMJJ-UHFFFAOYSA-N C(C(=C)C)(=O)OC(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.P(=O)(O)(O)O Chemical compound C(C(=C)C)(=O)OC(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.P(=O)(O)(O)O NDERRIHSWCOMJJ-UHFFFAOYSA-N 0.000 description 1
- 102000013392 Carboxylesterase Human genes 0.000 description 1
- 108010051152 Carboxylesterase Proteins 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002949 hemolytic effect Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 210000001616 monocyte Anatomy 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/12—Esters of phosphoric acids with hydroxyaryl compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a kind of method and devices quickly recycling triphenyl phosphate from discarded circuit board, including solvent heat treatment reactor, it is characterised in that：Rotary stainless steel net cover is equipped in the solvent heat treatment reactor, rotary stainless steel net cover is connected with rotating speed controller；Temperature controller and pressure regulation instrument are connected on solvent heat treatment reactor, solvent heat treatment reactor bottom is equipped with valve, valve lower section is equipped with isopropanol receiving bottle.The invention also discloses the methods of the device used.Method of the present invention compared with prior art in the present invention is a kind of environmental-friendly method, almost non-secondary pollution.The device and method of triphenyl phosphate is recycled using the slave discarded circuit board in the present invention, reaction time can foreshorten to 40 minutes than existing method, organic efficiency is increased to 99.6%, and purity reaches 99.8%, to realize the efficient quick recycling of triphenyl phosphate in discarded circuit board.
Description
Technical field
The invention belongs to field of environment engineering, be related to a kind of method quickly recycling triphenyl phosphate from discarded circuit board and
Device.
Background technology
In recent years, the use due to brominated flame-retardant in printed wiring board is restricted, and organophosphorous fire retardant is printing
Usage amount in wiring board manufacture rapidly rises.Early in 2004, the yield of global organophosphorous fire retardant just accounted for fire retardant total yield
The 14% of amount.In general, organophosphorous fire retardant is used as chemical addition agent and is not bonded with polymer material matrix,
Therefore, if mishandling, organophosphorous fire retardant can migrate into environment and generate threat to human health.Such as extensively
For the triphenyl phosphate of wiring board plasticiser and fire retardant, be effective inhibitor of human blood monocyte carboxy-lesterase simultaneously
With hemolytic toxicity.Therefore, it is current electricity for the processing of the safe retrieving of the huge triphenyl phosphate of content in discarded circuit board
Sub- waste field urgent problem.
Currently, the technical method disposed for triphenyl phosphate in discarded circuit board having disclosed include landfill, burn,
Pyrolysis and mechanical means.The above method there are problems that triphenyl phosphate can not be recycled and generate secondary pollution.2014,
Cong-Cong Zhang et al. disclose a kind of side recycling triphenyl phosphate in discarded circuit board using methanol solvate thermal process
Method (Chemical Engineering Journal 240 (2014) 10-15).This method is specific as follows：It is used as back using methanol
Medium is received, the temperature for controlling solvent methanol is 90 degree, and the reaction time is 120 minutes, and the solid-to-liquid ratio of discarded circuit board and methanol is
1:10, it centrifuges after reaction, it is to recycle that solvent, which mutually uses rotary evaporation recycling design methanol, remaining solid product,
Triphenyl phosphate.This method is 84.4% for the organic efficiency of triphenyl phosphate in discarded circuit board, purity 93.4%.
As can be seen that methanol solvate thermal process disclosed in Cong-Cong Zhang et al. returns triphenyl phosphate in discarded circuit board
Rate of producing effects is still relatively low (only 84.4%), and purity is not high (only 93.4%) yet, takes longer (120 minutes).
Invention content
To solve the problems, such as current discarded circuit board processing, it is quick from discarded circuit board that the present invention provides one kind
Recycle the method and device of triphenyl phosphate.
The present invention adopts the following technical scheme that realization：
A method of triphenyl phosphate quickly being recycled from discarded circuit board, is included the following steps：
Step 1) it will be crushed containing the abandoned printed circuit board of triphenyl phosphate fire retardant, then by the waste-line after crushing
Road plate is put into stainless steel net cover；Stainless (steel) wire is placed in solvent heat treatment reactor, is then reacted to solvent heat treatment
It is added isopropanol in device, the solid-to-liquid ratio of discarded circuit board and isopropanol is 1:4~1:10g/mL；Rotate stainless steel net cover, rotating speed
For 30-60rpm；It is 90 DEG C in solvent heat treatment reactor temperature, under conditions of pressure is 1.5Mpa, reacts 30-50 minutes；
Step 2) after reaction, stainless steel net cover stops rotating, and opens reactor bottom valve, and reaction product is turned
It moves in isopropanol receiving bottle, recycling isopropanol is evaporated at a temperature of 85 DEG C using Rotary Evaporators to get to solid phosphoric acid
Triphenylmethyl methacrylate；The isopropanol that recycling is obtained again is used for solvent heat treatment unit.
Further to improve, the solid-to-liquid ratio of the discarded circuit board and isopropanol is 1:7g/mL；The rotating speed of stainless steel net cover
For 30-60rpm；It it is 40 minutes in the solvent heat treatment reaction time.
A kind of device quickly recycling triphenyl phosphate from discarded circuit board, including solvent heat treatment reactor, it is described molten
Agent, which is heat-treated in reactor, is equipped with rotary stainless steel net cover, and rotary stainless steel net cover is connected with rotating speed controller；Solvent heat
It is connected with temperature controller and pressure regulation instrument in treatment reactor, solvent heat treatment reactor bottom is equipped with valve, under valve
Side is equipped with isopropanol receiving bottle.
The beneficial effects of the invention are as follows：
The method in the present invention is a kind of environmental-friendly method compared with prior art, almost non-secondary pollution.Using
The device and method of slave discarded circuit board recycling triphenyl phosphate in the present invention, reaction time can shorten than existing method
To 40 minutes, organic efficiency was increased to 99.6%, and purity reaches 99.8%, to realize triphenyl phosphate in discarded circuit board
Efficient quick recycling.
Description of the drawings
Fig. 1 is the structural schematic diagram of embodiment 1.
Fig. 2 is the process flow chart of embodiment 4.
Specific implementation mode
Below in conjunction with attached drawing, technical scheme in the embodiment of the invention is clearly and completely described.
Embodiment 1
A kind of device quickly recycling triphenyl phosphate from discarded circuit board as shown in Figure 1, including solvent heat treatment are anti-
Device 1 is answered, rotary stainless steel net cover 2 is equipped in the solvent heat treatment reactor 1, rotary stainless steel net cover 2, which is connected with, to be turned
Fast controller 3；Temperature controller 4 and pressure regulation instrument 5, solvent heat treatment reactor 1 are connected on solvent heat treatment reactor 1
Bottom is equipped with valve 6, and 6 lower section of valve is equipped with isopropanol receiving bottle 7.
Embodiment 2：
The abandoned printed circuit board containing triphenyl phosphate fire retardant is ground into graininess first, size is to be not less than
The mesh size size of stainless steel net cover 2 is limited, then granular discarded circuit board is put into stainless steel net cover 2, after will not
Rust steel mesh is placed in solvent heat treatment reactor 1, and isopropanol is then added into solvent heat treatment reactor, and isopropanol is added
Amount presses the solid-to-liquid ratio 1 of certain discarded circuit board and isopropanol:4g/mL is controlled, and reaction temperature is controlled by temperature controller 4
90 degrees Celsius, reaction pressure is controlled by pressure regulation instrument 5 in 1.5Mpa, and the rotating speed of stainless steel net cover 2 passes through rotating speed controller 3
Control controls in 0rpm, reaction time at 30 minutes, and after reaction, stainless steel net cover stops rotating, and temperature of reactor is dropped
To room temperature, reactor bottom valve 6 is opened, and take isopropanol solvent phase product, isopropanol molten by the reception of isopropanol receiving bottle 7
Agent phase product recycles isopropanol solvent at 85 degree using Rotary Evaporators and is back to solvent heat treatment unit.Rotary evaporation
Obtained solid product is triphenyl phosphate powder after removing isopropanol, is weighed to it and purity analysis, and heavy by its
It measures and calculates its organic efficiency with the content of triphenyl phosphate in first original circuit plate.The experimental results showed that：Triphenyl phosphate recycles
Efficiency is 85.2%, and purity reaches 98%.
Embodiment 3：
The abandoned printed circuit board containing triphenyl phosphate fire retardant is ground into graininess first, size is to be not less than
The mesh size size of stainless steel net cover 2 is limited, then granular discarded circuit board is put into stainless steel net cover 2, after will not
Rust steel mesh is placed in solvent heat treatment reactor 1, and isopropanol is then added into solvent heat treatment reactor, and isopropanol is added
Amount presses the solid-to-liquid ratio 1 of certain discarded circuit board and isopropanol:4g/mL is controlled, and reaction temperature is controlled by temperature controller 4
90 degree, reaction pressure is controlled by pressure regulation instrument 5 in 1.5Mpa, and the rotating speed of stainless steel net cover 2 is controlled by rotating speed controller 3
In 30rpm, direction of rotation is suitable, counterclockwise, and the reaction time controlled at 30 minutes, and after reaction, stainless steel net cover stops
Temperature of reactor is down to room temperature by rotation, opens reactor bottom valve 6, and take isopropanol by the reception of isopropanol receiving bottle 7
Solvent phase product, isopropanol solvent phase product recycle isopropanol solvent at 85 degree using Rotary Evaporators and are back to solvent
Thermal treatment unit.Obtained solid product is triphenyl phosphate powder after rotary evaporation removes isopropanol, it weigh and
Purity analysis, and its organic efficiency is calculated by the content of triphenyl phosphate in its weight and first original circuit plate.Experimental result
Show：Triphenyl phosphate organic efficiency is 92.4%, and purity reaches 98%.
Embodiment 4：
As shown in Fig. 2, the abandoned printed circuit board containing triphenyl phosphate fire retardant is ground into graininess, ruler first
The very little mesh size size with not less than stainless steel net cover 2 is limited, then granular discarded circuit board is put into stainless steel net cover 2
In, after stainless (steel) wire is placed in solvent heat treatment reactor 1, isopropanol then is added into solvent heat treatment reactor,
Quantity of isopropanol presses the solid-to-liquid ratio 1 of certain discarded circuit board and isopropanol:7g/mL is controlled, and reaction temperature passes through temperature
The control of instrument 4 is controlled at 90 degree, reaction pressure is controlled by pressure regulation instrument 5 in 1.5Mpa, and the rotating speed of stainless steel net cover 2 passes through rotating speed
For the control of controller 3 in 45rpm, direction of rotation is suitable, counterclockwise, and the reaction time controlled at 40 minutes, after reaction, stainless
Steel mesh set stops rotating, and temperature of reactor is down to room temperature, opens reactor bottom valve 6, and connect by isopropanol receiving bottle 7
Collect isopropanol solvent phase product, isopropanol solvent phase product using Rotary Evaporators recycled at 85 degree isopropanol solvent and by its
It is back to solvent heat treatment unit.It is triphenyl phosphate powder that rotary evaporation, which removes the solid product obtained after isopropanol, to it
It is weighed and purity analysis, and is imitated by the content of triphenyl phosphate in its weight and first original circuit plate to calculate its recycling
Rate.The experimental results showed that：Triphenyl phosphate organic efficiency is 99.6%, and purity reaches 99.8%.
Embodiment 5：
The abandoned printed circuit board containing triphenyl phosphate fire retardant is ground into graininess first, size is to be not less than
The mesh size size of stainless steel net cover 2 is limited, then granular discarded circuit board is put into stainless steel net cover 2, after will not
Rust steel mesh is placed in solvent heat treatment reactor 1, and isopropanol is then added into solvent heat treatment reactor, and isopropanol is added
Amount presses the solid-to-liquid ratio 1 of certain discarded circuit board and isopropanol:10g/mL is controlled, and reaction temperature is controlled by temperature controller 4
At 90 degree, reaction pressure is controlled by pressure regulation instrument 5 in 1.5Mpa, and the rotating speed of stainless steel net cover 2 is controlled by rotating speed controller 3
System is in 60rpm, and direction of rotation is suitable, counterclockwise, and the reaction time controlled at 50 minutes, and after reaction, stainless steel net cover stops
Spin-ended turn, temperature of reactor is down to room temperature, opens reactor bottom valve 6, and isopropyl is taken by the reception of isopropanol receiving bottle 7
Alcoholic solvent phase product, isopropanol solvent phase product recycle isopropanol solvent at 85 degree using Rotary Evaporators and are back to molten
Agent thermal treatment unit.It is triphenyl phosphate powder that rotary evaporation, which removes the solid product obtained after isopropanol, is weighed to it
And purity analysis, and its organic efficiency is calculated by the content of triphenyl phosphate in its weight and first original circuit plate.Experiment knot
Fruit shows：Triphenyl phosphate organic efficiency is 99.6%, and purity reaches 99.8%.
Claims (2)
1. a kind of method quickly recycling triphenyl phosphate from discarded circuit board, which is characterized in that include the following steps：
Step 1) it will be crushed containing the abandoned printed circuit board of triphenyl phosphate fire retardant, then by the discarded circuit board after crushing
It is put into stainless steel net cover；Stainless (steel) wire is placed in solvent heat treatment reactor, then into solvent heat treatment reactor
The solid-to-liquid ratio of addition isopropanol, discarded circuit board and isopropanol is 1:4~1:10g/mL；Rotate stainless steel net cover, rotating speed 30-
60rpm；It is 90 DEG C in solvent heat treatment reactor temperature, under conditions of pressure is 1.5Mpa, reacts 30-50 minutes；
Step 2) after reaction, stainless steel net cover stops rotating, and opens reactor bottom valve, reaction product is transferred to
In isopropanol receiving bottle, recycling isopropanol is evaporated at a temperature of 85 DEG C using Rotary Evaporators to get to solid phosphoric acid triphen
Ester；The isopropanol that recycling is obtained again is used for solvent heat treatment unit.
2. the method for quickly recycling triphenyl phosphate from discarded circuit board as described in claim 1, which is characterized in that described useless
The solid-to-liquid ratio for abandoning wiring board and isopropanol is 1:7g/mL；The rotating speed of stainless steel net cover is 30-60rpm；It is reacted in solvent heat treatment
Time is 40 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610391938.XA CN106008595B (en) | 2016-06-03 | 2016-06-03 | A kind of method and device quickly recycling triphenyl phosphate from discarded circuit board |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610391938.XA CN106008595B (en) | 2016-06-03 | 2016-06-03 | A kind of method and device quickly recycling triphenyl phosphate from discarded circuit board |
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| Publication Number | Publication Date |
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| CN106008595A CN106008595A (en) | 2016-10-12 |
| CN106008595B true CN106008595B (en) | 2018-08-21 |
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| CN201610391938.XA Expired - Fee Related CN106008595B (en) | 2016-06-03 | 2016-06-03 | A kind of method and device quickly recycling triphenyl phosphate from discarded circuit board |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107236000B (en) * | 2017-06-06 | 2018-12-07 | 池正伟 | The recovery method of triphenyl phosphate |
| CN109395667B (en) * | 2017-08-18 | 2021-08-03 | 上海浦景化工技术股份有限公司 | Axial-radial reactor for synthesizing dimethyl oxalate through CO carbonylation coupling |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102532588A (en) * | 2012-01-05 | 2012-07-04 | 中国科学院生态环境研究中心 | Method for separating flame retardant from waste electronic and electric product plastic |
| CN202725605U (en) * | 2012-06-14 | 2013-02-13 | 中国科学院生态环境研究中心 | Hydrothermal treatment device for discarded printed circuit boards |
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