CN106927695A - The low temperature closed-loop process technique of discarded glass - Google Patents
The low temperature closed-loop process technique of discarded glass Download PDFInfo
- Publication number
- CN106927695A CN106927695A CN201710203766.3A CN201710203766A CN106927695A CN 106927695 A CN106927695 A CN 106927695A CN 201710203766 A CN201710203766 A CN 201710203766A CN 106927695 A CN106927695 A CN 106927695A
- Authority
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- China
- Prior art keywords
- glass
- discarded
- low temperature
- defoamer
- acid
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- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 65
- 239000011521 glass Substances 0.000 title claims abstract description 60
- 239000003365 glass fiber Substances 0.000 claims abstract description 34
- 239000013530 defoamer Substances 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 239000004094 surface-active agent Substances 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 14
- 229910052593 corundum Inorganic materials 0.000 claims description 14
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 14
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 150000007522 mineralic acids Chemical class 0.000 claims description 12
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Chemical compound [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 7
- 239000010922 glass waste Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- CMMUKUYEPRGBFB-UHFFFAOYSA-L dichromic acid Chemical compound O[Cr](=O)(=O)O[Cr](O)(=O)=O CMMUKUYEPRGBFB-UHFFFAOYSA-L 0.000 claims description 5
- 230000002000 scavenging effect Effects 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- -1 acrylic ester Chemical class 0.000 claims description 4
- 239000003822 epoxy resin Substances 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical group CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000004913 activation Effects 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 230000031709 bromination Effects 0.000 claims description 2
- 238000005893 bromination reaction Methods 0.000 claims description 2
- 150000002170 ethers Chemical class 0.000 claims description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 2
- 150000002466 imines Chemical class 0.000 claims description 2
- 238000005470 impregnation Methods 0.000 claims description 2
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 229920001568 phenolic resin Polymers 0.000 claims description 2
- 239000005011 phenolic resin Substances 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims description 2
- SFVFIFLLYFPGHH-UHFFFAOYSA-M stearalkonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 SFVFIFLLYFPGHH-UHFFFAOYSA-M 0.000 claims description 2
- 229920006305 unsaturated polyester Polymers 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 6
- 238000011161 development Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000005265 energy consumption Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 230000008961 swelling Effects 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- 241001062472 Stokellia anisodon Species 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000007380 fibre production Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- XQSBLCWFZRTIEO-UHFFFAOYSA-N hexadecan-1-amine;hydrobromide Chemical class [Br-].CCCCCCCCCCCCCCCC[NH3+] XQSBLCWFZRTIEO-UHFFFAOYSA-N 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 235000019738 Limestone Nutrition 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 241001417490 Sillaginidae Species 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229910052903 pyrophyllite Inorganic materials 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/70—Cleaning, e.g. for reuse
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/64—Drying; Dehydration; Dehydroxylation
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/66—Chemical treatment, e.g. leaching, acid or alkali treatment
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Geochemistry & Mineralogy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Processing Of Solid Wastes (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Surface Treatment Of Glass Fibres Or Filaments (AREA)
Abstract
Present invention relates particularly to a kind of scrap glass fiber treatment technique.The low temperature closed-loop process technique of discarded glass of the invention, including：（1）The discarded glass of cleaning, dries；（2）Crush, obtain glass powder；（3）Impregnating active treatment；（4）Catalyst, defoamer, surfactant and solvent are placed in reactor and process；（5）Dry, calcining prepares glass fibre.The method of the present invention has exemplary role in field of the same trade, while also having huge Industry Effect power, can bring considerable economic benefit.The method of the present invention meets green production and sustainable development strategies, also complies with resource reclaim and recycles policy, and DEVELOPMENT PROSPECT is wide.
Description
Technical field
Present invention relates particularly to a kind of scrap glass fiber treatment technique.
Background technology
Glass fibre is a kind of Inorganic Non-metallic Materials of excellent performance, with quartz sand, pyrophyllite, lime stone, boric acid etc.
Natural inorganic non-metallic ore is raw material, and by certain formula, through high temperature melting, wire drawing, doff etc., several technique is made,
With high temperature resistant, anti-corruption, heat-insulated, tensile strength is high, and electrical insulating property waits well excellent properties, in electronic apparatus, auto industry, aviation
Space flight, wind-power electricity generation and biomedicine field are used widely.But glass fibre belongs to fragile material, in order to strengthen its
Mechanical property complies with process requirements, needs to be soaked in its surface coated glass fiber in the drawing process of production glass fibre
Profit agent.Size can not only effectively lubricating glass fiber surface, moreover it is possible to by hundreds of or even thousands of glass monofilament integrated
Beam, does not bond mutually between precursor after precursor is wound in cake.Increase glass fibre simultaneously soft during post-processing
It is soft, reduce mechanical wear.Generally, the compositions such as film forming agent, coupling agent, lubricant, antistatic additive can be added in size, in glass
Glass fiber surface forms a labyrinth layer for having concentration gradient.
Glass fiber waste silk is the industrial tailing of generation in glass fibre production, is a kind of solid waste, and China is annual
3~50,000 tons of waste silks for scribbling different type size will be produced, is a greatly burden for enterprise, for society
Environmental pollution can more be caused.Choosing buried mode earliest carries out the treatment of waste silk, and the processing method causes the wave in a large amount of farmlands
Take and pollute.As the control that Environmental is protected is more and more stricter, buried mode is eliminated completely, glass fibre production
Enterprise needs the new method of searching badly to solve the problems, such as scrap glass fiber contamination.Most cheap, most environmentally friendly mode is at present
Glass fibre is melted down again, but because the ratio when presence of size makes glass waste silk melt down again is unable to reach production
Demand, therefore need to carry out the removal of size before melting down.The method of tradition removal size is high-temperature calcination, and temperature reaches 1400
DEG C, the method energy consumption it is higher and produce waste gas very big harm is caused to environment.Therefore seek energy consumption it is low, it is pollution-free removal leaching
Profit agent method turns into glass fibre enterprise problem in the urgent need to address.
The content of the invention
It is low, pollution-free removal size to useless the invention provides a kind of energy consumption in order to solve above-mentioned technical problem
Abandon the low temperature closed-loop process technique of glass.
Closed-loop process technique of the present invention, refers to take some specific handling process aborning, by what is produced
Recovery and reuse of waste, externally without discharge（Zero-emission）, pollution-free, the process that realization is recycled, so that reducing energy consumption, saves
Cost, and favorable environment.
The low temperature closed-loop process technique of discarded glass of the invention, including：
（1）The discarded glass of cleaning, dries；
（2）Crush, obtain glass powder；
（3）The treatment of inorganic acid impregnating active；
（4）Catalyst, defoamer, surfactant and solvent are placed in reactor and process；
（5）Dry, calcining prepares glass fibre.
Discarded glass involved in the present invention includes epoxide resin type glass, unsaturated polyester type glass, acrylic ester type
The discarded glasses such as glass, phenolic resin type glass, polyurethane-type glass.
Discarded glass being cleaned using the method being cleaned by ultrasonic, supersonic frequency is 30~100KHz, scavenging period is 1~
15min；Glass waste silk after cleaning is in dry 2~10h at 80~120 DEG C.
Dried discarded glass is cut into short silk of the length less than 2mm, air-flow micronizer, air velocity is sent into
It is the hypervelocity swirling eddy of more than 1.5MHZ, discharge pressure is 0.5~1.2MPa.
Inorganic acid impregnation process step specifically, pickling bath liquor pH value be 1~5, inorganic acid be hydrochloric acid, sulfuric acid, nitric acid,
The mixture of one or more in phosphoric acid, hypochlorous acid, dichromic acid, perchloric acid, the addition of inorganic acid is glass powder gross weight
The 3~10% of amount, the impregnating active time is 6~10h.
Above-mentioned catalyst includes Al2O3, KNO3/Al2O3, KOH/Al2O3, NaOH/ Al2O3, LiOH/ Al2O3, CsOH/
Al2O3, NaOH, KOH, LiOH, at least one in CsOH；
Solvent includes at least one in water, lower alcohol, organic alkane, ethers；
Surfactant is stearic acid, neopelex, stearyl dimethyl benzyl ammonium chloride, cetyl bromination
At least one in ammonium, sorbierite surfactant；
Defoamer is organic silicon defoamer, polyethers defoamer, silicon and ether grafting class defoamer, defoamer containing amine, imines
At least one of class defoamer and amide-type defoamer；
Glass powder after activation：Catalyst：Solvent：Surfactant：The quality parts ratio of defoamer is 20~30：3~8：80~
100：0.5~1.2：0.1~0.8.
Preferably,（4）In reaction condition it is as follows：Under the conditions of 50~120 DEG C, pressure be 0.5~1MPa, stirring 4~
12h, stir speed (S.S.) is 1000~3000r/min.
（5）Middle glass fibre evaporation, after reclaiming solvent for use, 1h~5h is dried at 100~250 DEG C, and kiln is returned after drying
Calcining prepares glass fibre.
The present invention employs lossless, green, environment-friendly treating process for glass fiber treating compound removal.At present rarely have similar to
This technology is realized industrialization by the documents and materials report of the inventive method, Ye Weiyou enterprises, and the method for the present invention is led in the same industry
There is exemplary role in domain, while also having huge Industry Effect power, considerable economic benefit can be brought.The present invention
Method meet green production and sustainable development strategies, also comply with resource reclaim and recycle policy, DEVELOPMENT PROSPECT is wide.
Brief description of the drawings
Fig. 1 is SEM measurement results after the inventive method treatment glass waste silk；
Fig. 2 is present invention process flow chart.
Specific embodiment
Come to be further described the present invention with reference to the accompanying drawings and detailed description, so as to the technology of this area
Personnel know more about the present invention, but with this do not limit the present invention.
Heretofore described " part ", unless otherwise specified, refers both to parts by weight；
Embodiment 1
The low temperature closed-loop process technique of epoxide resin type glass fiber waste silk, comprises the following steps：
（1）Epoxide resin type glass fiber waste silk is cleaned by ultrasonic, supersonic frequency is 70KHz, scavenging period is 15min,
Cleaning at 80 DEG C after drying 5h；
（2）Dried discarded glass cuts into the short silk of length 1mm or so, and air-flow ultramicro grinding is sent under air-flow drive
Machine, air velocity is the hypervelocity swirling eddy of more than 1.8MHz, and discharge pressure is 0.6MPa, and 200 mesh sieves are crossed after crushing；
（3）Discarded glass powder after by sieving is placed in impregnating active 8 hours or so in inorganic acid, and inorganic acid accounts for glass powder gross weight
5% or so of amount, selected inorganic acid is 1.5mol/L nitric acid and 0.8mol/L dichromic acid mixed solutions, the effect of inorganic acid soak
It is to make the size generation on glass powder surface swelling, destroys its cross-linked structure between glass fibre；
Nitric acid：Dichromic acid（V/V）=1：2；
（4）It is filtered to remove acid solution（Acid solution is reusable）, filter residue is obtained, 15 weight portion LiOH/ are added in 100 weight portion filter residues
Al2O3With KOH mixtures, LiOH/ Al2O3It is 1 with the weight ratio of KOH：2,2.5 weight portion stearic acid, 1 weight portion organosilicon disappears
Infusion（Foam can be produced during stirring reaction）With 400 parts by weight of cyclohexane solvents, various raw materials are well mixed and are poured into instead
Kettle is answered, mixing speed is 2500r/min, at 50 °C, 6h is reacted under conditions of 0.5MPa；
（5）Separation of solid and liquid after 6h, liquid carries out solvent recovery in being directly entered triple effect evaporation tower, after solid dries 2h at 100 °C
Directly return kiln and smelt calcining.
Be glass waste silk ESEM comparison diagram after treatment shown in accompanying drawing 2, it is untreated as shown in Figure 2 before glass waste silk
Because the parcel of size shows smooth, and after size is divested completely, in glass surface residual fraction size
Relic, the rough glass surface of exposing surface after washing can remove most sizes after implementing technique of the invention
Remove.
Embodiment 2
The low temperature closed-loop process technique of polyester-type glass fiber waste silk, comprises the following steps：
（1）Polyester-type glass fiber waste silk is cleaned by ultrasonic, supersonic frequency is 90KHz, scavenging period is 10min, is cleaned
3h is dried after 90 °C；
（2）Dried discarded glass cuts into short silk of the length less than 2mm, and air-flow ultramicro grinding is sent under air-flow drive
Machine, air velocity is the hypervelocity swirling eddy of more than 1.8MHz, and discharge pressure is 1MPa, and 200 mesh sieve are crossed after crushing；
（3）Discarded glass powder after by sieving be placed in account for glass powder gross weight 10% 10 parts of 0.2-0.8mol/L perchloric acid and
10h is soaked in 20 parts of 2-3mol/L sulfuric acid mixed solutions, makes the size generation on glass powder surface swelling, destroy itself and glass
Cross-linked structure between fiber；
（4）It is filtered to remove acid solution（Acid solution is reusable）, 20 parts of CsOH, 2 parts of cetyl ammonium bromides are added in 100 parts of filter residues
With the mixture of sorbierite（The weight ratio of cetyl ammonium bromide and sorbierite is 4：1）, 1.2 parts of organosilicons and polyether antifoam agent
Mixture（The weight ratio of organosilicon and polyethers is 3：1）With 200 parts of dichloromethane solvents, poured into after various raw materials are well mixed
Reactor, mixing speed is 2500r/min, at 80 DEG C, 2h is reacted under conditions of 0.5MPa；
（5）Separation of solid and liquid after 2h, liquid carries out solvent recovery in being directly entered triple effect evaporation tower, and solid dries 1.5h at 150 DEG C
Kiln is directly returned afterwards smelts calcining.
Elementary analysis Comparative result table
Carry out processing the determination of elemental analysis of forward and backward glass waste silk by taking case study on implementation 2 as an example, analyze the data in above table,
Draw following conclusion：Untreated glass surface is because the presence of organic type size, and the content of C, H, N is higher.Closed in low temperature
After ring PROCESS FOR TREATMENT, the content of C, H, N is rapidly reduced, it was demonstrated that the size on surface is substantially all to be divested.Compared to conventional high-temperature
The processing method of calcining, method provided by the present invention has saved energy consumption without high-temperature process, and agents useful for same is recyclable heavy
Multiple to utilize, per ton cost can be controlled in less than 500 yuan.
Embodiment 3
The low temperature closed-loop process technique of acrylic ester type glass fiber waste silk, comprises the following steps：
（1）Acrylic ester type glass fiber waste silk is cleaned by ultrasonic, supersonic frequency is 80KHz, scavenging period is 12min,
Cleaning dries 3h after 90 °C；
（2）Dried discarded glass cuts into short silk of the length less than 2mm, and air-flow ultramicro grinding is sent under air-flow drive
Machine, air velocity is the hypervelocity swirling eddy of more than 1.8MHz, and discharge pressure is 0.5MPa, and 200 mesh sieve are crossed after crushing；
（3）Discarded glass powder after by sieving be placed in account for 10 part of 20% hydrochloric acid of glass powder gross weight 3%, 15% dichromic acid and
8h is soaked in 15% perchloric acid solution（Bichromate solution is 1 with the volume ratio of perchloric acid solution：1）, make the leaching on glass powder surface
Profit agent generation is swelling, destroys its cross-linked structure between glass fibre；
（4）It is filtered to remove acid solution（Acid solution is reusable）, 10 parts of KOH, 4 parts of sorbierites, 1.5 parts of acyls are added in 100 parts of filter residues
Amine defoamer（Foam is produced during stirring reaction）With 250 parts of cyclohexane solvents, various raw materials are well mixed and pour into reaction
Kettle, mixing speed is 3000r/min, at 60 °C, 4h is reacted under conditions of 1MPa；
（5）Separation of solid and liquid after 4h, liquid carries out solvent recovery in being directly entered triple effect evaporation tower, after solid dries 4h at 100 °C
Directly return kiln and smelt calcining.Kiln calcining can be directly returned after dried process and prepares glass fibre, discard glass surface size
Clearance can reach more than 98%, the loss late of selected solvent is less than 1 ‰.
Claims (8)
1. the low temperature closed-loop process technique of glass is discarded, including：
（1）The discarded glass of cleaning, dries；
（2）Crush, obtain glass powder；
（3）The treatment of inorganic acid impregnating active；
（4）Catalyst, defoamer, surfactant and solvent are placed in reactor and process；
（5）Dry, calcining prepares glass fibre.
2. the low temperature closed-loop process technique of glass is discarded as claimed in claim 1, it is characterised in that discarded glass includes epoxy
Resin type glass, unsaturated polyester type glass, acrylic ester type glass, phenolic resin type glass, polyurethane-type glass etc. are discarded
Glass.
3. the low temperature closed-loop process technique of glass is discarded as claimed in claim 1, it is characterised in that using the side being cleaned by ultrasonic
To discarded glass cleaning, supersonic frequency is 30~100KHz to method, and scavenging period is 1~15min；Glass waste silk after cleaning is in 80
5~10h is dried at~120 DEG C.
4. the low temperature closed-loop process technique of glass is discarded as claimed in claim 1, it is characterised in that by dried discarded glass
Fibre cuts into short silk of the length less than 2mm, sends into air-flow micronizer, and air velocity is the hypervelocity rotary pneumatic of more than 1.5MHZ
Stream, discharge pressure is 0.5~1.2MPa.
5. the low temperature closed-loop process technique of glass is discarded as claimed in claim 1, it is characterised in that inorganic acid impregnation process is walked
Suddenly specifically, the pH value of pickling bath liquor is 1~5, inorganic acid is hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, hypochlorous acid, dichromic acid, chlorine high
At least one in acid, inorganic acid addition is the 3~10% of glass powder gross weight, and the impregnating active time is 6~10h.
6. the low temperature closed-loop process technique of glass is discarded as claimed in claim 1, it is characterised in that
Catalyst includes Al2O3, KNO3/Al2O3, KOH/Al2O3, NaOH/ Al2O3, LiOH/ Al2O3, CsOH/ Al2O3, NaOH,
At least one in KOH, LiOH, CsOH；
Solvent includes at least one in water, lower alcohol, organic alkane, ethers；
Surfactant is stearic acid, neopelex, stearyl dimethyl benzyl ammonium chloride, cetyl bromination
At least one in ammonium, sorbierite surfactant；
Defoamer is organic silicon defoamer, polyethers defoamer, silicon and ether grafting class defoamer, defoamer containing amine, imines
At least one of class defoamer and amide-type defoamer；
Glass powder after activation：Catalyst：Solvent：Surfactant：The quality parts ratio of defoamer is 20~30：3~8：80~
100：0.5~1.2：0.1~0.8.
7. the low temperature closed-loop process technique of glass is discarded as claimed in claim 1, it is characterised in that（4）In reaction condition
It is as follows：Under the conditions of 50~120 DEG C, pressure is 0.5~1MPa, stirs 4~12h, and stir speed (S.S.) is 1000~3000r/min.
8. the low temperature closed-loop process technique of glass is discarded as claimed in claim 1, it is characterised in that warp（4）Glass after treatment
Glass fiber evaporates, and after reclaiming solvent for use, 1h~5h is dried at 100~250 DEG C, and dried glass fibre returns kiln calcining system
Standby glass fibre.
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| CN108975680A (en) * | 2018-09-18 | 2018-12-11 | 重庆国际复合材料股份有限公司 | A kind of glass fibre operates on the recovery method of silk |
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