CN1919402A - Supercritical carbon dioxide extraction recovery device for waste electric appliance combustion inhibitor and method thereof - Google Patents
Supercritical carbon dioxide extraction recovery device for waste electric appliance combustion inhibitor and method thereof Download PDFInfo
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- CN1919402A CN1919402A CNA2006100939354A CN200610093935A CN1919402A CN 1919402 A CN1919402 A CN 1919402A CN A2006100939354 A CNA2006100939354 A CN A2006100939354A CN 200610093935 A CN200610093935 A CN 200610093935A CN 1919402 A CN1919402 A CN 1919402A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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Abstract
The invention discloses a supercritical carbon dioxide extraction recycling method and device of fire retardant in the waste electric appliance, which is characterized by the following: connecting carbon dioxide container exit with low-temperature cooling liquid circulating pump inlet, connecting low-temperature cooling liquid circulating pump exit with high pressure pump inlet, connecting high pressure pump exit with abstractor inlet, setting abstractor in the constant temperature heater, connecting abstractor exit with ultraviolet split-field photometer and separating collector inlet through backpressure valve, connecting separating collector outlet with metering gauge, setting separating collector in the cooler. the recycling method comprises the following steps: grinding waste electric appliance, sieving, loading in the extract, starting circulating pump, opening outlet valve of reserving tank, starting high-pressure pump, entering carbon dioxide in the extract through filter, observing extracting condition through ultraviolet split-field photometer, dissolving extracted fire retardant in the separating collector to recycle toluene.
Description
Technical field
The present invention relates to a kind of supercritical carbon dioxide extracting recovery technology, especially relate to the supercritical carbon dioxide extraction recovery device and the method thereof of fire retardant in a kind of waste electric appliance.
Background technology
Along with the quickening that electronic product updates, scrapping that the processing of household electrical appliances, discarded computer and communication apparatus and resource utilize again is one of various countries' urgent task in this century.At present the focus of various countries remains to avoiding environmental pollution to handle electron wastes, and less input for the resource recycling of electron wastes.The conventional method of handling solid waste mainly adopts the method for landfill and burning, but these methods make poisonous and harmful substance contaminated soil, underground water and air in the electron wastes.Simultaneously, the recycling of failing of a large amount of metals that contain in the electron wastes and the fire retardant of high added value causes the huge wasting of resources.In addition, owing to the proportion that plastics in the electronic product are shared is increasing, adopt landfill disposal to be difficult to degraded; Adopt burning disposal, then enter in soil and the air because the existence of high molecular polymer and fire retardant etc. easily generates carcinogens such as dioxin and furans.At present, some developed countries pay much attention to for the recycling of precious metal in the electron wastes, developed industrial treatment equipment, the main employing becomes fine particle to the electron wastes mechanical crushing, adopt method separating metal and plastics such as screening, density separation, magnetic force and electrostatic separation then, and then reclaim metal.But the residual plastic particle still is used as discarded object landfill or burning because can't be re-used as the raw material of producing electrical equipment uses, and causes environmental pollution.And contain 15%～30% high added value fire retardant in these plastics, if recycling will bring considerable economic, social benefit and ecological benefits.
Supercritical fluid technique is the new and high technology of " environmental friendliness " of growing up over nearly 30 years.Supercritical fluid is owing to have special physicochemical character, is the research of current research a focus, particularly supercritical liquid extraction technique and realizes industrialization the earliest.Supercritical liquid extraction technique has the advantage that the traditional extraction method is not had, and it changes the character of solvent easily by regulating pressure and temperature, the control extraction selectivity, and rate of extraction is fast.At present, carbon dioxide be use in the supercritical liquid extraction technique at most, solvent the most widely, have low price, inertia, advantage such as nontoxic.Supercritical carbon dioxide density is big, and is strong to the organic matter solvability, can operate near under the room temperature, separates thorough and easy with extraction product.Therefore, supercritical carbon dioxide extraction method progressively is applied in fields such as chemical industry, medicine, food, light industry, material, environmental protection, and is in the high speed development.
The research of supercritical carbon dioxide extracting separating solids mixture has many reports, set up relevant kinetic model for mechanism of mass transfer, many researchs have obtained many complex system equilibriums under the high pressure, also carry out simultaneously the basic study on thermodynamic model of supercritical carbon dioxide extracting process, obtained many basic datas.The molecular structure of carbon dioxide has determined it that the liposoluble substance of hydro carbons and low pole is had a good solvability, the addition type bromine system or the phosphorus flame retardant that mainly contain in the resinous material of electronic product, major part is the ester type organic, these fire retardants generally have higher solubility in supercritical carbon dioxide, therefore, adopt this based flame retardant of supercritical carbon dioxide extracting can receive good effect.At present, both at home and abroad for the relevant report of this type of organic bromine system and phosphorus flame retardant extraction research seldom, and the basic data of being correlated with quite lacks.Gamse, (Gamse T, Steinkellner F, Marr R, et al.Solubility studies oforganic flame retardants in supercritical CO such as T.
2Ind.Eng.Chem.Res.2000,39:4888) bromide fire retardant: HBCD (HBCD) and the solubility of TBBA (tetrabromobisphenol A) in supercritical carbon dioxide have been studied, temperature range is 25～100 ℃, pressure is 200～500bar, and experimental result is used the Chrastil formula simulate, obtained coincideing preferably the result.Bunte, (Bunte G, Hardle Th, Krause H, et al.Extraction ofbrominated flame retardants with supercritical CO such as G.
2Process Technol.Proc.1996,12:535) studied employing supercritical carbon dioxide extraction typical bromide fire retardant: HBCD (HBCD) from simulation magnesium sulfate mixture, the technical process of TBBA (tetrabromobisphenol A) and TBPA has been investigated the influence for the fire retardant rate of recovery of extraction temperature, extracting pressure and extraction time.Draw from extraction process: under 80 ℃ of 350bar conditions, when the extraction time reached 30 minutes, the rate of recovery of TBBA reached more than 70%, so extraction efficiency is higher; On the other hand, from experimental result as can be known, temperature is little for the influence of the rate of recovery of fire retardant, and pressure influence highly significant, when pressure arrived 350bar greatly, the rate of recovery of TBBA obviously improved, and reached more than 70%.But this research is not studied the influence of the rate of recovery the granular size of mixture, and, only studied the simulation mixture, do not study the fire retardant extract and separate in the true waste electric appliance goods.In addition, more than research all is confined to be subjected to use in the research of bromide fire retardant of restriction, not at present and the extraction of the following main phosphorus flame retardant of using reclaim and do not study.
Summary of the invention
The objective of the invention is to the problem that exists in the fire retardant recovery technology in the existing waste electric appliance, the supercritical carbon dioxide extracting recovery method and the device thereof of fire retardant in a kind of waste electric appliance is provided.
The technical solution used in the present invention is to adopt the resin material of actual waste electrical equipment as raw material for this reason, and the employing carbon dioxide is an extractant, reclaims the addition type organic fire-retardant in the waste electrical equipment resin material, to obtain the high fire retardant rate of recovery.
The supercritical carbon dioxide extraction recovery device of fire retardant is provided with carbon dioxide storage tank, cryogenic liquid circulating pump, high-pressure pump, extractor, online uv-spectrophotometric instrument, counterbalance valve, separated and collected device, cooler, flowmeter etc. in the waste electric appliance of the present invention.The outlet of solvent carbon dioxide storage tank connects the cryogenic liquid pump entry, the cold air outlet of cryogenic liquid circulating pump connects the inlet of high-pressure pump, the bottom inlet of extractor is received in the high-pressure pump outlet, extractor is located in the constent temperature heater and by constent temperature heater and is heated, extractor outlet is connected on line uv-spectrophotometric instrument and by connecing the import of separated and collected device behind the counterbalance valve, the outlet of separated and collected device connects flowmeter, and the separated and collected device is located in the cooler.
Outlet and asking of cryogenic liquid pump entry at carbon dioxide storage tank are provided with valve and filter, and the inlet of valve connects the carbon dioxide storage tank outlet, and filter inlet connects valve export and cryogenic liquid pump inlet respectively with outlet.Can connect Pressure gauge in the extractor outlet, pressure is regulated by high-pressure pump and counterbalance valve.On constent temperature heater and cooler, be respectively equipped with temperature controller, to regulate the temperature on constent temperature heater and the cooler.
Package unit can adopt high pressure resistant stainless steel material to make.
The supercritical carbon dioxide extracting recovery method of fire retardant the steps include: in the waste electric appliance of the present invention
1) pulverizes and sieves out the printed circuit board (PCB) or the electrical equipment resin material particle of different-grain diameter scope earlier, as standby raw material;
2) get same size particles, in the extractor of packing into, start the cryogenic liquid circulating pump, open the carbon dioxide storage tank outlet valve, start high-pressure pump;
3) carbon dioxide enters extractor through filter by the high-pressure pump pressurization, and extraction kettle pressure is controlled by counterbalance valve;
4) by the constent temperature heater heating and by temperature controller control extraction kettle temperature;
5) observe the extraction situation by online uv-spectrophotometric instrument;
6) fire retardant that extracts reclaims with the toluene dissolving in the separated and collected device of cooling, the carbon dioxide that flows out from the separated and collected device is by the flowmeter metered flow, extract solution carries out qualitative and quantitative analysis with gas chromatograph-mass spectrometer (GC-MS) and gas chromatograph, after extraction was finished, weighing was also write down the weight of remaining solid powder in the extractor.Can obtain wherein organophosphor or the rate of recovery of bromide fire retardant be 70%～100%.
Printed circuit board (PCB) or its particle size range of electrical equipment resin material particle of pulverizing and sieving out the different-grain diameter scope are 0.1～2.8mm.The carbon dioxide flow of described carbon dioxide storage tank is 0.035～0.16g/s, and the extraction time is 0.5～4h.
The described pressure that enters extractor by high-pressure pump pressurization is 10～50MPa.Control extraction kettle temperature is 313～373K.
In step 5), after meeting the requirements of pressure and temperature, observe the extraction situation by online uv-spectrophotometric instrument, keep stable carbon dioxide flow simultaneously.
Extractant can adopt carbon dioxide, and the collection solvent is an organic solvent, can be selected from toluene, acetone, ether, chloroform etc.
The printed circuit board (PCB) of raw material employing waste electric appliance and resin case material etc., callable fire retardant mainly contains:
Triphenyl phosphate TPP, tricresyl phosphate TCP, di(2-ethylhexyl)phosphate phenyl (tert-butyl-phenyl) ester DPBPP, phosphoric acid hexichol (toluene) ester DPTP, diphenyl 2 ethylhexyl phosphate DPOP, tricresyl phosphate (2-fourth oxygen ethyl) ester TBEP, tributyl phosphate TBP, tricresyl phosphate (dimethylbenzene) ester TXP, tricresyl phosphate (β, β "-two chloro isopropyls) ester TDCPP; tricresyl phosphate (β-chloroethyl) ester TCEP, triethyl phosphate TEP, tricresyl phosphate (cumenyl) ester TIPPP; HBCD HBCD; tetrabromobisphenol A TBBA, octabromodiphenyl ether OBDPO, 2; 4-dibromophenol DBP; poly-dibromobenzene aether PBO, deca-BDE DBDPO, tribromo-benzene ylmethyl acrylate TBPMA, decabrominated dipheny base ethane, penta-BDE PBDPO and tetrabromophthalic anhydride TBPA etc.
The organophosphor that the present invention adopts supercritical carbon dioxide extracting to reclaim in the waste electric appliance is and bromide fire retardant, respectively to waste printed circuit board and casing resin material etc. after low-temperature grinding, the particle that sieves out different-grain diameter is as raw material, by the supercritical CO 2 extraction technology process, investigate of the influence of technological parameters such as pressure, temperature, extraction time, carbon dioxide flow, grain diameter respectively, reclaim the optimum process condition of fire retardant in the waste electric appliance to determine supercritical carbon dioxide extracting for the organophosphor system and the bromide fire retardant rate of recovery.
The present invention is mainly used in waste electric appliance recycling field, especially is applied to the renewable resources that waste electric appliance reclaims the toner behind the metal and handles, and is more suitable for the recycling of the waste material of electrical equipment and fitment material production process.
Outstanding advantage of the present invention is to adopt the eco-friendly supercritical carbon dioxide extracting isolation technics of green non-pollution, realizes the extraction separation process three-waste free discharge.Simultaneously,, low price nontoxic, tasteless, reusable edible as the carbon dioxide of extractant, the critical-temperature of carbon dioxide be 31 ℃ near normal temperature, therefore, extraction process is saved energy consumption.In addition, the solvent carbon dioxide only separates with the solute fire retardant and is promptly separated fully by reducing pressure, and technical process is simple, processing ease.
Effect of the present invention can be checked by the fire retardant rate of recovery that extraction separation process obtains.The rate of recovery of fire retardant mainly is stressed, the control of temperature, extraction time, granular size and carbon dioxide flow.The rate of recovery of organic phosphorus flame retardant reaches as high as 98% in the raw material waste electric appliance, and the rate of recovery of organic bromine flame retardant reaches as high as 100%, the organic efficiency height.Simultaneously, the flame retardant products purity height of recovery does not have any dissolvent residual, can directly utilize again.
Description of drawings
Fig. 1 is that the structure of the supercritical carbon dioxide extraction recovery device of fire retardant in the waste electric appliance is formed schematic diagram.
The specific embodiment
The detailed retracting device embodiment of the supercritical carbon dioxide extraction recovery device of fire retardant as shown in Figure 1 in the waste electric appliance of the present invention, the outlet of solvent carbon dioxide storage tank 1 connects a valve V, carbon dioxide by valve V enters the filter 11 that is installed on the pipeline, is cooled to subzero through cryogenic liquid circulating pump 2 then and enters high-pressure pump 3.High-pressure pump 3 outlets are connected to extractor 4 bottom inlets, extractor 4 is by constent temperature heater 5 heating of its peripheral parcel, extractor 4 outlets connect online uv-spectrophotometric instrument 6, enter separated and collected device 8 by counterbalance valve 7 then and collect the fire retardant that reclaims, separated and collected device 8 outlet connection traffic meters 10 are measured its flow.
Meet Pressure gauge P in extractor 4 outlets, pressure is regulated by high-pressure pump 3 and counterbalance valve 7.On constent temperature heater 5 and cooler 9, be respectively equipped with temperature controller TC, to regulate the temperature on constent temperature heater and the cooler.
Package unit can adopt high pressure resistant stainless steel material to make.The printed circuit board (PCB) of raw material employing waste electric appliance and resin case material etc., extractant can adopt carbon dioxide, and the collection solvent is an organic solvent, can be selected from toluene, acetone, ether, chloroform etc.
Below provide the supercritical carbon dioxide extraction recovery device that utilizes fire retardant in the waste electric appliance and reclaim fire retardant in the waste electric appliance
Embodiment.
Embodiment 1: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.1mm of waste printed circuit board, pressure 20MPa, temperature 343K, extraction time 30min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 75%.
Embodiment 2: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 20MPa, temperature 343K, extraction time 30min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 60%.
Embodiment 3: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 1.5mm of waste printed circuit board, pressure 20MPa, temperature 343K, extraction time 30min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 29%.
Embodiment 4: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 2.8mm of waste printed circuit board, pressure 20MPa, temperature 343K, extraction time 30min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 8%.
Embodiment 5: waste printed circuit board, and the waste material of board production process, wherein fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) is provided by hitachi Co., Ltd..Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.1mm of waste printed circuit board, pressure 20MPa, temperature 343K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 86%.
Embodiment 6: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 1.5mm of waste printed circuit board, pressure 20MPa, temperature 343K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 39%.
Embodiment 7: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 2.8mm of waste printed circuit board, pressure 20MPa, temperature 343K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 18%.
Embodiment 8: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.1mm of waste printed circuit board, pressure 20MPa, temperature 343K, extraction time 120min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 98%.
Embodiment 9: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 20MPa, temperature 343K, extraction time 120min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 86%.
Embodiment 10: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 1.5mm of waste printed circuit board, pressure 20MPa, temperature 343K, extraction time 120min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 45%.
Embodiment 11: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 2.8mm of waste printed circuit board, pressure 20MPa, temperature 343K, extraction time 120min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 27%.
Embodiment 12: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 20MPa, temperature 313K, extraction time 60min, carbon dioxide flow 0.08g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 1%.
Embodiment 13: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 20MPa, temperature 323K, extraction time 60min, carbon dioxide flow 0.08g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 3%.
Embodiment 14: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 20MPa, temperature 333K, extraction time 60min, carbon dioxide flow 0.08g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 29%.
Embodiment 15: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 20MPa, temperature 343K, extraction time 60min, carbon dioxide flow 0.08g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 45%.
Embodiment 16: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 20MPa, temperature 313K, extraction time 60min, carbon dioxide flow 0.13g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 8%.
Embodiment 17: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 20MPa, temperature 323K, extraction time 60min, carbon dioxide flow 0.13g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 13%.
Embodiment 18: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 20MPa, temperature 333K, extraction time 60min, carbon dioxide flow 0.13g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 48%.
Embodiment 19: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 20MPa, temperature 343K, extraction time 60min, carbon dioxide flow 0.13g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 62%.
Embodiment 20: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 10MPa, temperature 313K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 5%.
Embodiment 21: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 15MPa, temperature 313K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 9%.
Embodiment 22: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 20MPa, temperature 313K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 14%.
Embodiment 23: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 25MPa, temperature 313K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 17%.
Embodiment 24: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 10MPa, temperature 323K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 14%.
Embodiment 25: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 15MPa, temperature 323K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 19%.
Embodiment 26: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 20MPa, temperature 323K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 24%.
Embodiment 27: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 25MPa, temperature 323K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 38%.
Embodiment 28: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 10MPa, temperature 333K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 36%.
Embodiment 29: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 15MPa, temperature 333K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 39%.
Embodiment 30: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 20MPa, temperature 333K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 56%.
Embodiment 31: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 25MPa, temperature 333K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 74%.
Embodiment 32: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 10MPa, temperature 343K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 43%.
Embodiment 33: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 15MPa, temperature 343K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 49%.
Embodiment 34: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 20MPa, temperature 343K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 74%.
Embodiment 35: waste printed circuit board, and the waste material of board production process, fire retardant TPP (triphenyl phosphate) content: 16.7wt% (weight) wherein, Co., Ltd. provides by hitachi.Toluene is analyzed purely, and purity 〉=99.8% is by providing with light pure chemistry Industrial Co., Ltd.Operating condition: the grain diameter 0.4mm of waste printed circuit board, pressure 25MPa, temperature 343K, extraction time 60min, carbon dioxide flow 0.16g/s.Obtaining wherein, the rate of recovery of fire retardant TPP (triphenyl phosphate) is 93%.
Embodiment 36: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant TBBA (tetrabromobisphenol A) content: 17wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 313K, extraction time 240min, carbon dioxide flow 0.035g/s.Obtaining wherein, the rate of recovery of fire retardant TBBA (tetrabromobisphenol A) is 31%.
Embodiment 37: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant TBBA (tetrabromobisphenol A) content: 17wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 333K, extraction time 240min, carbon dioxide flow 0.035g/s.Obtaining wherein, the rate of recovery of fire retardant TBBA (tetrabromobisphenol A) is 65%.
Embodiment 38: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant TBBA (tetrabromobisphenol A) content: 17wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.035g/s.Obtaining wherein, the rate of recovery of fire retardant TBBA (tetrabromobisphenol A) is 91%.
Embodiment 39: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant TBBA (tetrabromobisphenol A) content: 17wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 373K, extraction time 240min, carbon dioxide flow 0.035g/s.Obtaining wherein, the rate of recovery of fire retardant TBBA (tetrabromobisphenol A) is 98%.
Embodiment 40: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant TBBA (tetrabromobisphenol A) content: 17wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 313K, extraction time 240min, carbon dioxide flow 0.07g/s.Obtaining wherein, the rate of recovery of fire retardant TBBA (tetrabromobisphenol A) is 60%.
Embodiment 41: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant TBBA (tetrabromobisphenol A) content: 17wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 333K, extraction time 240min, carbon dioxide flow 0.07g/s.Obtaining wherein, the rate of recovery of fire retardant TBBA (tetrabromobisphenol A) is 92%.
Embodiment 42: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant TBBA (tetrabromobisphenol A) content: 17wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.07g/s.Obtaining wherein, the rate of recovery of fire retardant TBBA (tetrabromobisphenol A) is 98%.
Embodiment 43: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant TBBA (tetrabromobisphenol A) content: 17wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 373K, extraction time 240min, carbon dioxide flow 0.07g/s.Obtaining wherein, the rate of recovery of fire retardant TBBA (tetrabromobisphenol A) is 100%.
Embodiment 44: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant TBBA (tetrabromobisphenol A) content: 17wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 313K, extraction time 240min, carbon dioxide flow 0.1g/s.Obtaining wherein, the rate of recovery of fire retardant TBBA (tetrabromobisphenol A) is 79%.
Embodiment 45: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant TBBA (tetrabromobisphenol A) content: 17wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 333K, extraction time 240min, carbon dioxide flow 0.1g/s.Obtaining wherein, the rate of recovery of fire retardant TBBA (tetrabromobisphenol A) is 97%.
Embodiment 46: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant TBBA (tetrabromobisphenol A) content: 17wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.1g/s.Obtaining wherein, the rate of recovery of fire retardant TBBA (tetrabromobisphenol A) is 100%.
Embodiment 47: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant TBBA (tetrabromobisphenol A) content: 17wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 373K, extraction time 240min, carbon dioxide flow 0.1g/s.Obtaining wherein, the rate of recovery of fire retardant TBBA (tetrabromobisphenol A) is 100%.
Embodiment 48: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant TBBA (tetrabromobisphenol A) content: 17wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 313K, extraction time 240min, carbon dioxide flow 0.13g/s.Obtaining wherein, the rate of recovery of fire retardant TBBA (tetrabromobisphenol A) is 85%.
Embodiment 49: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant TBBA (tetrabromobisphenol A) content: 17wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 333K, extraction time 240min, carbon dioxide flow 0.13g/s.Obtaining wherein, the rate of recovery of fire retardant TBBA (tetrabromobisphenol A) is 99%.
Embodiment 50: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant TBBA (tetrabromobisphenol A) content: 17wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.13g/s.Obtaining wherein, the rate of recovery of fire retardant TBBA (tetrabromobisphenol A) is 100%.
Embodiment 51: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant TBBA (tetrabromobisphenol A) content: 17wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 373K, extraction time 240min, carbon dioxide flow 0.13g/s.Obtaining wherein, the rate of recovery of fire retardant TBBA (tetrabromobisphenol A) is 100%.
Embodiment 52: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 313K, extraction time 240min, carbon dioxide flow 0.035g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 37%.
Embodiment 53: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 313K, extraction time 240min, carbon dioxide flow 0.07g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 52%.
Embodiment 54: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 313K, extraction time 240min, carbon dioxide flow 0.1g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 60%.
Embodiment 55: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 313K, extraction time 240min, carbon dioxide flow 0.13g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 64%.
Embodiment 56: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 333K, extraction time 240min, carbon dioxide flow 0.035g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 68%.
Embodiment 57: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 333K, extraction time 240min, carbon dioxide flow 0.07g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 85%.
Embodiment 58: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 333K, extraction time 240min, carbon dioxide flow 0.1g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 92%.
Embodiment 59: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 333K, extraction time 240min, carbon dioxide flow 0.13g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 96%.
Embodiment 60: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.035g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 91%.
Embodiment 61: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.07g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 97%.
Embodiment 62: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.1g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 98%.
Embodiment 63: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.13g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 99%.
Embodiment 64: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 373K, extraction time 240min, carbon dioxide flow 0.035g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 99%.
Embodiment 65: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 373K, extraction time 240min, carbon dioxide flow 0.07g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 100%.
Embodiment 66: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 373K, extraction time 240min, carbon dioxide flow 0.1g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 100%.
Embodiment 67: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 50MPa, temperature 373K, extraction time 240min, carbon dioxide flow 0.13g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 100%.
Embodiment 68: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 20MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.035g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 35%.
Embodiment 69: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 20MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.07g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 53%.
Embodiment 70: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 20MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.1g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 67%.
Embodiment 71: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 20MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.13g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 72%.
Embodiment 72: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 30MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.035g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 70%.
Embodiment 73: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 30MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.07g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 82%.
Embodiment 74: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 30MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.1g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 88%.
Embodiment 75: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 30MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.13g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 90%.
Embodiment 76: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 40MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.035g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 88%.
Embodiment 77: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 40MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.07g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 99%.
Embodiment 78: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 40MPa, temperature 353K, extraction time 240min, carbon dioxide flow 0.1g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 100%.
Embodiment 79: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.25mm of waste electric appliance resin material, pressure 40MPa, temperature 353K, extraction time 240min, three carbonoxide flow 0.13g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 100%.
Embodiment 80: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.7mm of waste electric appliance resin material, pressure 50MPa, temperature 373K, extraction time 240min, carbon dioxide flow 0.035g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 69%.
Embodiment 81: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.7mm of waste electric appliance resin material, pressure 50MPa, temperature 373K, extraction time 240min, carbon dioxide flow 0.056g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 77%.
Embodiment 82: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.7mm of waste electric appliance resin material, pressure 50MPa, temperature 373K, extraction time 240min, carbon dioxide flow 0.07g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 80%.
Embodiment 83: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 0.7mm of waste electric appliance resin material, pressure 50MPa, temperature 373K, extraction time 240min, carbon dioxide flow 0.08g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 82%.
Embodiment 84: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 1.0mm of waste electric appliance resin material, pressure 50MPa, temperature 373K, extraction time 240min, carbon dioxide flow 0.035g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 34%.
Embodiment 85: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 1.0mm of waste electric appliance resin material, pressure 50MPa, temperature 373K, extraction time 240min, carbon dioxide flow 0.056g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 41%.
Embodiment 86: waste electric appliance casing resin material, collect voluntarily, wherein fire retardant HBCD (HBCD) content: 22.4wt% (weight).Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 1.0mm of waste electric appliance resin material, pressure 50MPa, temperature 373K, extraction time 240min, carbon dioxide flow 0.07g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 45%.
Embodiment 87:L waste electric appliance casing resin material is collected, wherein fire retardant HBCD (HBCD) content: 224wt% (weight) voluntarily.Toluene is analyzed purely, and purity 〉=99.5% is provided by Chemical Reagent Co., Ltd., Sinopharm Group.Operating condition: the grain diameter 1.0mm of waste electric appliance resin material, pressure 50MPa, temperature 373K, extraction time 240min, carbon dioxide flow 0.08g/s.Obtaining wherein, the rate of recovery of fire retardant HBCD (HBCD) is 49%.
Claims (10)
1. the supercritical carbon dioxide extraction recovery device of fire retardant in the waste electric appliance is characterized in that being provided with carbon dioxide storage tank, cryogenic liquid circulating pump, high-pressure pump, extractor, online uv-spectrophotometric instrument, counterbalance valve, separated and collected device, cooler and flowmeter; The outlet of carbon dioxide storage tank connects the cryogenic liquid pump entry, the cold air outlet of cryogenic liquid circulating pump connects the inlet of high-pressure pump, the bottom inlet of extractor is received in the high-pressure pump outlet, extractor is located in the constent temperature heater and by constent temperature heater and is heated, extractor outlet is connected on line uv-spectrophotometric instrument and by connecing the import of separated and collected device behind the counterbalance valve, the outlet of separated and collected device connects flowmeter, and the separated and collected device is located in the cooler.
2. the supercritical carbon dioxide extraction recovery device of fire retardant in the waste electric appliance as claimed in claim 1, it is characterized in that between the outlet of carbon dioxide storage tank and cryogenic liquid pump entry, being provided with valve and filter, the inlet of valve connects the carbon dioxide storage tank outlet, and filter inlet connects valve export and cryogenic liquid pump inlet respectively with outlet.
3. the supercritical carbon dioxide extraction recovery device of fire retardant in the waste electric appliance as claimed in claim 1 is characterized in that connecing Pressure gauge in the extractor outlet.
4. the supercritical carbon dioxide extraction recovery device of fire retardant in the waste electric appliance as claimed in claim 1 is characterized in that being respectively equipped with temperature controller on constent temperature heater and cooler.
5. the supercritical carbon dioxide extracting recovery method of fire retardant in the waste electric appliance is characterized in that the steps include:
1) pulverizes and sieves out the printed circuit board (PCB) or the electrical equipment resin material particle of different-grain diameter scope earlier, as standby raw material;
2) get same size particles, in the extractor of packing into, start the cryogenic liquid circulating pump, open the carbon dioxide storage tank outlet valve, start high-pressure pump;
3) carbon dioxide enters extractor through filter by the high-pressure pump pressurization, rising pressure to 10～50MPa, and extraction kettle pressure is controlled by counterbalance valve;
4) by the constent temperature heater heating and by temperature controller control extraction kettle temperature;
5) observe the extraction situation by online uv-spectrophotometric instrument;
6) fire retardant that extracts reclaims with the toluene dissolving in the separated and collected device of cooling, the carbon dioxide that flows out from the separated and collected device is by the flowmeter metered flow, extract solution carries out qualitative and quantitative analysis with gas chromatograph-mass spectrometer (GC-MS) and gas chromatograph, after extraction was finished, weighing was also write down the weight of remaining solid powder in the extractor.
6. the supercritical carbon dioxide extracting recovery method of fire retardant in the waste electric appliance as claimed in claim 5, printed circuit board (PCB) or its particle size range of electrical equipment resin material particle of it is characterized in that pulverizing and sieve out the different-grain diameter scope are 0.1～2.8mm.
7. the supercritical carbon dioxide extracting recovery method of fire retardant in the waste electric appliance as claimed in claim 5, the carbon dioxide flow that it is characterized in that described carbon dioxide storage tank is 0.035～0.16g/s, the extraction time is 0.5～4h.
8. the supercritical carbon dioxide extracting recovery method of fire retardant in the waste electric appliance as claimed in claim 5 is characterized in that the described pressure that enters extractor by high-pressure pump pressurization is 10～50MPa.
9. the supercritical carbon dioxide extracting recovery method of fire retardant in the waste electric appliance as claimed in claim 5, it is characterized in that controlling the extraction kettle temperature is 313～373K.
10. the supercritical carbon dioxide extracting recovery method of fire retardant in the waste electric appliance as claimed in claim 5, it is characterized in that in step 5), after meeting the requirements of pressure and temperature, observe the extraction situation by online uv-spectrophotometric instrument, keep stable carbon dioxide flow simultaneously.
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