CN117509685A - Technology for preparing sodium carbonate from industrial salt by using membrane method - Google Patents
Technology for preparing sodium carbonate from industrial salt by using membrane method Download PDFInfo
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- CN117509685A CN117509685A CN202311747820.2A CN202311747820A CN117509685A CN 117509685 A CN117509685 A CN 117509685A CN 202311747820 A CN202311747820 A CN 202311747820A CN 117509685 A CN117509685 A CN 117509685A
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- sodium carbonate
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- industrial salt
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 title claims abstract description 93
- 239000012528 membrane Substances 0.000 title claims abstract description 46
- 229910000029 sodium carbonate Inorganic materials 0.000 title claims abstract description 42
- 150000003839 salts Chemical class 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000005516 engineering process Methods 0.000 title claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000178 monomer Substances 0.000 claims abstract description 35
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000004005 microsphere Substances 0.000 claims abstract description 28
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims description 57
- 238000002156 mixing Methods 0.000 claims description 40
- 238000001035 drying Methods 0.000 claims description 36
- 230000003301 hydrolyzing effect Effects 0.000 claims description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 22
- 239000000919 ceramic Substances 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 16
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 16
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 16
- 239000000839 emulsion Substances 0.000 claims description 16
- 229910000077 silane Inorganic materials 0.000 claims description 16
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(iii) oxide Chemical compound O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 11
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical group COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000005119 centrifugation Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000012065 filter cake Substances 0.000 claims description 9
- 239000011148 porous material Substances 0.000 claims description 9
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 8
- 239000003995 emulsifying agent Substances 0.000 claims description 8
- 230000001804 emulsifying effect Effects 0.000 claims description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims description 8
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 8
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 8
- OTYBJBJYBGWBHB-UHFFFAOYSA-N trimethylsilyl prop-2-enoate Chemical compound C[Si](C)(C)OC(=O)C=C OTYBJBJYBGWBHB-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 229910001938 gadolinium oxide Inorganic materials 0.000 claims description 7
- 229940075613 gadolinium oxide Drugs 0.000 claims description 7
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 7
- 239000003999 initiator Substances 0.000 claims description 7
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 6
- GUCYFKSBFREPBC-UHFFFAOYSA-N [phenyl-(2,4,6-trimethylbenzoyl)phosphoryl]-(2,4,6-trimethylphenyl)methanone Chemical group CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C(=O)C1=C(C)C=C(C)C=C1C GUCYFKSBFREPBC-UHFFFAOYSA-N 0.000 claims description 4
- BOQSSGDQNWEFSX-UHFFFAOYSA-N propan-2-yl 2-methylprop-2-enoate Chemical compound CC(C)OC(=O)C(C)=C BOQSSGDQNWEFSX-UHFFFAOYSA-N 0.000 claims description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 3
- 125000002816 methylsulfanyl group Chemical group [H]C([H])([H])S[*] 0.000 claims description 3
- 125000004573 morpholin-4-yl group Chemical group N1(CCOCC1)* 0.000 claims description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000006227 byproduct Substances 0.000 abstract description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 6
- 239000013049 sediment Substances 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 239000004408 titanium dioxide Substances 0.000 abstract description 3
- 239000003463 adsorbent Substances 0.000 abstract description 2
- 238000000975 co-precipitation Methods 0.000 abstract description 2
- 239000013081 microcrystal Substances 0.000 abstract description 2
- 230000006911 nucleation Effects 0.000 abstract description 2
- 238000010899 nucleation Methods 0.000 abstract description 2
- 125000005375 organosiloxane group Chemical group 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 33
- 235000017550 sodium carbonate Nutrition 0.000 description 28
- 229940001593 sodium carbonate Drugs 0.000 description 26
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 239000000460 chlorine Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000000356 contaminant Substances 0.000 description 3
- MQRJBSHKWOFOGF-UHFFFAOYSA-L disodium;carbonate;hydrate Chemical compound O.[Na+].[Na+].[O-]C([O-])=O MQRJBSHKWOFOGF-UHFFFAOYSA-L 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229940076133 sodium carbonate monohydrate Drugs 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000003373 anti-fouling effect Effects 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical class O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- LWRBVKNFOYUCNP-UHFFFAOYSA-N 2-methyl-1-(4-methylsulfanylphenyl)-2-morpholin-4-ylpropan-1-one Chemical compound C1=CC(SC)=CC=C1C(=O)C(C)(C)N1CCOCC1 LWRBVKNFOYUCNP-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- NBFQLHGCEMEQFN-UHFFFAOYSA-N N.[Ni] Chemical compound N.[Ni] NBFQLHGCEMEQFN-UHFFFAOYSA-N 0.000 description 1
- RAWPGIYPSZIIIU-UHFFFAOYSA-N [benzoyl(phenyl)phosphoryl]-phenylmethanone Chemical group C=1C=CC=CC=1C(=O)P(=O)(C=1C=CC=CC=1)C(=O)C1=CC=CC=C1 RAWPGIYPSZIIIU-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000909 electrodialysis Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 238000009285 membrane fouling Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 150000003388 sodium compounds Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/22—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a technology for preparing sodium carbonate from industrial salt by using a membrane method, belonging to the technical field of byproduct industrial salt treatment; the invention takes away and disperses nucleation centers or microcrystals of at least one scaling compound when in use, so that scaling sediment on the surface of equipment can be avoided, and the co-precipitation of the sediment can be promoted when the rare earth oxide nanocrystalline, titanium dioxide, organosiloxane and acrylic acid monomer are mixed with water easy to scale, and the organic-inorganic composite nanometer hybrid microsphere can be used as an adsorbent or a carrier; the yield of the sodium carbonate prepared by the technical scheme of the invention is 88.51 percent, and the purity is more than 99.9 percent.
Description
Technical Field
The invention relates to the technical field of byproduct industrial salt treatment, in particular to a technology for preparing sodium carbonate from industrial salt by a membrane method.
Background
Sodium carbonate is one of the basic industrial raw materials, is used for manufacturing other sodium compounds, is widely used in industries such as metallurgy, papermaking, glass, ceramics, foods, dyes, detergents and the like and daily life, and plays a vital role in national economy.
CN201510851242.6: a process for preparing sodium carbonate by utilizing byproduct industrial salt belongs to the technical field of byproduct industrial salt treatment, and comprises the following steps: preparing the byproduct industrial salt into saturated brine, and filtering the saturated brine through an activated carbon filter; introducing ammonia gas at a rate of 0.1-0.5L/min at 20-30deg.C, and introducing carbon dioxide gas at a rate of 0.2-0.7L/min, and reacting until the crystal solid is not increased; cooling the obtained reaction liquid to 10-15 ℃, and then separating by using a centrifugal machine to obtain a solid; and (5) obtaining solid through thermal decomposition, and obtaining sodium carbonate and carbon dioxide gas. The invention carries out resource treatment on the byproduct industrial salt, reduces the content of organic impurities in the finished product, and can ensure the treatment effect of the byproduct industrial salt to the maximum extent.
CN200610135336.4: a method for preparing sodium carbonate relates to a process for preparing sodium carbonate by adopting an ammonia nickel method. The method for preparing the sodium carbonate has the advantages of readily available raw materials, small loss of medium ammonia and nickel, recycling, less pollution discharge, high product quality and controllable chlorine content within 0.1 percent. NiO is dissolved in CO 2 Mixing with ammonia water, absorbing ammonia to saturation, adding NaCl for double decomposition, filtering to separate Na 2 CO 3 Aqueous ammonia solution and Ni (NH) 3 ) 6 Cl 2 ；Na 2 CO 3 Distilling ammonia water solution to remove ammonia and filtering out precipitate Ni 2 (OH) 2 CO 3 Concentrating and crystallizing the filtrate to obtain the sodium carbonate product. Ni (NH) 3 ) 6 Cl 2 Heating to deaminate to obtain NiCl 2 ；NiCl 2 Heating and reacting with water vapor to obtain mixture of NiO and hydrogen chloride with water vapor or O in air 2 Reacting to obtain NiO and Cl 2 Recovering NiO from air mixture, condensing the mixture of hydrogen chloride and water vapor to obtain hydrochloric acid and Cl 2 And (3) freezing the mixture with air to obtain liquid chlorine.
CN86104760: the method for preparing pure carbon from natural sodium bicarbonate mineral sources by solution extraction comprises; (a) Contacting sodium hydroxide aqueous solution as solvent with underground deposit layer containing sodium bicarbonate to generate aqueous solution; (b) Extracting at least a portion of the mineral deposit to form an aqueous solution; (C) optionally concentrating the aqueous solution with a sodium carbonate source. (d) Selectively filtering the aqueous solution to remove entrained solids and insoluble materials; (e) Continuously crystallizing sodium carbonate monohydrate by evaporating water to produce a crystalline slurry; (f) Removing a portion of the crystallization slurry from the crystallizer process and separating the crystallized sodium carbonate monohydrate from the aqueous solution using a centrifuge and drying the sodium carbonate monohydrate.
In the prior art, a single membrane separation method is adopted, the concentration is not too high, the membrane pollution and scaling are serious, and the cost of a disc tube type reverse osmosis membrane is high; the use of electrodialysis alone is not only capital intensive, costly to operate, but ceramic membranes have been used to effectively treat water with greater amounts of contaminants by using high crossover flow rates that continually sweep away the contaminants during use. This cross flow significantly increases energy consumption and wear due to solids flowing through the ceramic shortens the useful life of the membrane, resulting in higher overall system and operating costs and reduced rates of removal of target contaminants. The ceramic membranes used in these heavily contaminated waters have a relatively high energy consumption and a relatively short service life.
Disclosure of Invention
A first object of the present invention is to provide a technique for preparing soda ash from industrial salt by a membrane process, which reduces membrane fouling deposits.
The second object of the invention is to provide a method for preparing the anti-scaling microsphere.
The first object of the invention is implemented by the following technical scheme:
s1: weighing 85-100 parts by mass of industrial salt and deionized water at 55-65 ℃, stirring and dissolving, and then adding 20-25 parts by mass of NaOH solution with the concentration of 0.08-0.1 mol/L;
s2: adding anti-scaling microspheres with the mass percentage content of 0.52-2.5 percent into the solution; stirring for 10-30 minutes at normal temperature, and then filtering the solution by using a ceramic membrane device;
s3: evaporating the filtered filtrate at 85-100deg.C for 5-8 hr, separating the obtained crystal slurry with centrifuge, and adding 25-45 parts saturated sodium carbonate solution into the centrifuge to wash filter cake;
s4: and drying the product obtained by centrifugation to obtain the high-purity sodium carbonate.
Preferably, the pore diameter of the ceramic membrane is 0.3-0.8 μm, and the running time is 2-6h.
Preferably, the drying temperature is 65-80 ℃ and the drying time is 1-4h.
The second object of the invention is implemented by the following technical scheme:
according to the parts by weight, uniformly mixing 5-12 parts of butyl titanate hydrolytic sol and 20-32 parts of silane hydrolytic sol, stirring for 2-5 hours, then adding 0.25-0.6 part of rare earth oxide nanocrystalline, stirring for reaction for 24-48 hours, then adding 3-6 parts of acrylic acid monomer pre-emulsion and 0.15-0.38 part of photoinitiator, uniformly stirring, controlling the temperature to 40-60 ℃ under ultraviolet irradiation, stirring for reaction for 3-6 hours, centrifuging after the reaction is completed, washing, and drying to obtain the anti-scaling microspheres.
Preferably, the tetrabutyl titanate hydrosol is prepared by mixing tetrabutyl titanate, acetylacetone and pure water according to a molar ratio of 10:35-40:0.5-1.2, and stirring at 40-60deg.C for 1-3 hr.
Preferably, the silane hydrolytic sol is obtained by uniformly mixing methyltrimethoxysilane, acryloxytrimethylsilane, isopropanol and pure water according to a molar ratio of 1:1:2-6:6-8, adding 1-3% of hydrochloric acid, and carrying out hydrolysis reaction for 60-120min at 40-60 ℃.
Preferably, the acrylic acid monomer pre-emulsion is obtained by uniformly mixing acrylic acid monomer, emulsifier sodium dodecyl benzene sulfonate and pure water according to the mass ratio of 1:0.01-0.1:10-15, and then fully stirring and emulsifying.
Preferably, the acrylic monomer is methyl acrylate or isopropyl methacrylate or butyl methacrylate.
Preferably, the rare earth oxide nanocrystalline is obtained by mixing gadolinium oxide nanocrystalline and erbium oxide nanocrystalline according to a mass ratio of 1:0.8-1.6.
Preferably, the initiator is bis (2, 4, 6-trimethylbenzoyl) phenylphosphine oxide or 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-propanone or bisbenzoylphenylphosphine oxide.
The invention has the following beneficial effects:
compared with the prior art, the organic-inorganic composite nano hybrid microsphere prepared by rare earth oxide nanocrystalline, titanium dioxide, organic siloxane and acrylic acid monomer takes away and disperses nucleation centers or microcrystals of at least one scaling compound when in use, so that scaling sediment on the surface of equipment can be avoided, and when the rare earth oxide nanocrystalline, titanium dioxide, organic siloxane and acrylic acid monomer are mixed with water which is easy to scale, coprecipitation of the sediment can be promoted, and the organic-inorganic composite nano hybrid microsphere can be used as an adsorbent or a carrier.
After interaction of the anti-fouling microspheres with at least one fouling-forming fluid comprising at least one fouling compound, the adsorbed fouling material may remain suspended from the at least one anti-fouling material and separated from the fouling-forming fluid by conventional fluid/particle separation methods.
Detailed Description
The present invention will be described in further detail with reference to examples and embodiments. It should not be construed that the scope of the above subject matter of the present invention is limited to the following embodiments, and all techniques realized based on the present invention are within the scope of the present invention.
The soda ash detection methods prepared in the examples and comparative examples of the present invention were performed with reference to the standard GB 210-92.
Example 1
A technology for preparing sodium carbonate from industrial salt by using a membrane method comprises the following operation steps:
s1: 85g of industrial salt and deionized water with the temperature of 55 ℃ are weighed, stirred and dissolved, and then 20g of NaOH solution with the concentration of 0.08mol/L is added;
s2: adding anti-scaling microspheres with the mass percentage of 0.52 percent of the solution; stirring for 10 minutes at normal temperature, and then filtering the solution by using a ceramic membrane device;
s3: evaporating the filtered filtrate at 85 ℃ for 5 hours, separating the obtained crystal slurry in a centrifuge, and adding 25g of saturated sodium carbonate solution into the centrifuge to wash a filter cake;
s4: and drying the product obtained by centrifugation to obtain the high-purity sodium carbonate.
The pore diameter of the ceramic membrane is 0.3 μm, and the running time is 2h.
The drying temperature is 65 ℃ and the drying time is 1h.
The anti-scaling microsphere is prepared according to the following process steps:
uniformly mixing 5g of tetrabutyl titanate hydrolytic sol and 20g of silane hydrolytic sol, stirring for 2 hours, adding 0.25g of rare earth oxide nanocrystalline, stirring and reacting for 24 hours, adding 3g of acrylic acid monomer pre-emulsion and 0.15g of photoinitiator, uniformly stirring, controlling the temperature to 40 ℃ under ultraviolet irradiation, stirring and reacting for 3 hours, centrifuging after the reaction is completed, washing and drying to obtain the anti-scaling microsphere.
The tetrabutyl titanate hydrolytic sol is prepared by mixing tetrabutyl titanate, acetylacetone and pure water according to the molar ratio of 10:35:0.5 Stirring at 40 ℃ for 1h.
The silane hydrolytic sol is prepared by uniformly mixing methyltrimethoxysilane, acryloxytrimethylsilane, isopropanol and pure water according to a molar ratio of 1:1:2:6, adding 1% hydrochloric acid, and carrying out hydrolysis reaction at 40 ℃ for 60 min.
The acrylic acid monomer pre-emulsion is obtained by uniformly mixing an acrylic acid monomer, sodium dodecyl benzene sulfonate serving as an emulsifier and pure water according to a mass ratio of 1:0.01:10, and then fully stirring and emulsifying.
The acrylic acid monomer is methyl acrylate.
The rare earth oxide nanocrystalline is obtained by mixing gadolinium oxide nanocrystalline and erbium oxide nanocrystalline according to the mass ratio of 1:0.8.
The initiator is bis (2, 4, 6-trimethylbenzoyl) phenylphosphine oxide.
Example 2
A technology for preparing sodium carbonate from industrial salt by using a membrane method comprises the following operation steps:
s1: 90g of industrial salt and deionized water with the temperature of 60 ℃ are weighed, stirred and dissolved, and 22g of NaOH solution with the concentration of 0.09mol/L is added;
s2: adding anti-scaling microspheres with the mass percentage content of 1 percent into the solution; stirring for 15 minutes at normal temperature, and then filtering the solution by using a ceramic membrane device;
s3: evaporating the filtered filtrate at 90 ℃ for 6 hours, separating the obtained crystal slurry in a centrifuge, and adding 30g of saturated sodium carbonate solution into the centrifuge to wash a filter cake;
s4: and drying the product obtained by centrifugation to obtain the high-purity sodium carbonate.
The pore diameter of the ceramic membrane is 0.4 μm, and the running time is 3h.
The drying temperature is 70 ℃ and the drying time is 2h.
The anti-scaling microsphere is prepared according to the following process steps:
uniformly mixing 7g of tetrabutyl titanate hydrolytic sol and 25g of silane hydrolytic sol, stirring for 3 hours, adding 0.4g of rare earth oxide nanocrystalline, stirring for 30 hours, adding 4g of acrylic acid monomer pre-emulsion and 0.2g of photoinitiator, uniformly stirring, controlling the temperature to 45 ℃ under ultraviolet irradiation, stirring for 4 hours, centrifuging after the reaction is completed, washing, and drying to obtain the anti-scaling microspheres.
The tetrabutyl titanate hydrolytic sol is prepared by mixing tetrabutyl titanate, acetylacetone and pure water according to the molar ratio of 10:36:0.7 Stirring at 45 ℃ for 2 hours.
The silane hydrolytic sol is prepared by uniformly mixing methyltrimethoxysilane, acryloxytrimethylsilane, isopropanol and pure water according to a molar ratio of 1:1:3:7, adding 2% hydrochloric acid, and carrying out hydrolysis reaction for 80min at 45 ℃.
The acrylic acid monomer pre-emulsion is obtained by uniformly mixing an acrylic acid monomer, sodium dodecyl benzene sulfonate serving as an emulsifier and pure water according to a mass ratio of 1:0.04:12, and then fully stirring and emulsifying.
The acrylic acid monomer is isopropyl methacrylate.
The rare earth oxide nanocrystalline is gadolinium oxide nanocrystalline and erbium oxide nanocrystalline according to the mass ratio of 1:1, and mixing.
The light initiator is 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone.
Example 3
A technology for preparing sodium carbonate from industrial salt by using a membrane method comprises the following operation steps:
s1: weighing 95g of industrial salt and deionized water at 60 ℃, stirring and dissolving, and then adding 24g of NaOH solution with the concentration of 0.09 mol/L;
s2: adding anti-scaling microspheres with the mass percentage content of 2 percent into the solution; stirring for 25 minutes at normal temperature, and then filtering the solution by using a ceramic membrane device;
s3: evaporating the filtered filtrate at 95 ℃ for 7 hours, separating the obtained crystal slurry in a centrifuge, and adding 40g of saturated sodium carbonate solution into the centrifuge to wash a filter cake;
s4: and drying the product obtained by centrifugation to obtain the high-purity sodium carbonate.
The pore diameter of the ceramic membrane is 0.7 μm, and the running time is 5h.
The drying temperature is 75 ℃, and the drying time is 3 hours.
The anti-scaling microsphere is prepared according to the following process steps:
uniformly mixing 10g of tetrabutyl titanate hydrolytic sol and 30g of silane hydrolytic sol, stirring for 4 hours, adding 0.5g of rare earth oxide nanocrystalline, stirring and reacting for 45 hours, adding 5g of acrylic acid monomer pre-emulsion and 0.3g of photoinitiator, uniformly stirring, controlling the temperature to 55 ℃ under ultraviolet irradiation, stirring and reacting for 5 hours, centrifuging after the reaction is completed, washing and drying to obtain the anti-scaling microsphere.
The tetrabutyl titanate hydrolytic sol is prepared by mixing tetrabutyl titanate, acetylacetone and pure water according to the molar ratio of 10:3:8: stirring at 1, 55deg.C for 2h.
The silane hydrolytic sol is prepared by uniformly mixing methyltrimethoxysilane, acryloxytrimethylsilane, isopropanol and pure water according to a molar ratio of 1:1:5:7, adding 2% hydrochloric acid, and carrying out hydrolysis reaction for 100min at 55 ℃.
The acrylic acid monomer pre-emulsion is obtained by uniformly mixing an acrylic acid monomer, an emulsifier sodium dodecyl benzene sulfonate and pure water according to the mass ratio of 1:0.08:14, and then fully stirring and emulsifying.
The acrylic acid monomer is isopropyl methacrylate.
The rare earth oxide nanocrystalline is obtained by mixing gadolinium oxide nanocrystalline and erbium oxide nanocrystalline according to a mass ratio of 1:1.4.
The light initiator is 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone.
Example 4
A technology for preparing sodium carbonate from industrial salt by using a membrane method comprises the following operation steps:
s1: 100g of industrial salt and deionized water with the temperature of 65 ℃ are weighed, stirred and dissolved, and then 25g of NaOH solution with the concentration of 0.1mol/L is added;
s2: adding anti-scaling microspheres with the mass percentage content of 2.5 percent into the solution; stirring for 30 minutes at normal temperature, and then filtering the solution by using a ceramic membrane device;
s3: evaporating the filtered filtrate at 100 ℃ for 8 hours, separating the obtained crystal slurry in a centrifuge, and adding 45g of saturated sodium carbonate solution into the centrifuge to wash a filter cake;
s4: and drying the product obtained by centrifugation to obtain the high-purity sodium carbonate.
The pore diameter of the ceramic membrane is 0.8 μm, and the running time is 6h.
The drying temperature is 80 ℃ and the drying time is 4 hours.
The anti-scaling microsphere is prepared according to the following process steps:
uniformly mixing 12g of tetrabutyl titanate hydrolytic sol and 32g of silane hydrolytic sol, stirring for 5 hours, adding 0.6g of rare earth oxide nanocrystalline, stirring and reacting for 48 hours, adding 6g of acrylic acid monomer pre-emulsion and 0.38g of photoinitiator, uniformly stirring, controlling the temperature to 60 ℃ under ultraviolet irradiation, stirring and reacting for 6 hours, centrifuging after the reaction is completed, washing and drying to obtain the anti-scaling microsphere.
The tetrabutyl titanate hydrolytic sol is prepared by mixing tetrabutyl titanate, acetylacetone and pure water according to the molar ratio of 10:40:1.2 Stirring at 60 ℃ for 3 hours.
The silane hydrolytic sol is prepared by uniformly mixing methyltrimethoxysilane, acryloxytrimethylsilane, isopropanol and pure water according to a molar ratio of 1:1:6:8, adding 3% hydrochloric acid, and carrying out hydrolysis reaction at 60 ℃ for 120 min.
The acrylic acid monomer pre-emulsion is obtained by uniformly mixing an acrylic acid monomer, sodium dodecyl benzene sulfonate serving as an emulsifier and pure water according to a mass ratio of 1:0.1:15, and then fully stirring and emulsifying.
The acrylic acid monomer is butyl methacrylate.
The rare earth oxide nanocrystalline is obtained by mixing gadolinium oxide nanocrystalline and erbium oxide nanocrystalline according to a mass ratio of 1:1.6.
The initiator is dibenzoyl phenyl phosphine oxide.
Comparative example 1
A technology for preparing sodium carbonate from industrial salt by using a membrane method comprises the following operation steps:
s1: 85g of industrial salt and deionized water with the temperature of 55 ℃ are weighed, stirred and dissolved, and then 20g of NaOH solution with the concentration of 0.08mol/L is added;
s2: filtering the solution by using a ceramic membrane device;
s3: evaporating the filtered filtrate at 85 ℃ for 5 hours, separating the obtained crystal slurry in a centrifuge, and adding 25g of saturated sodium carbonate solution into the centrifuge to wash a filter cake;
s4: and drying the product obtained by centrifugation to obtain the high-purity sodium carbonate.
The pore diameter of the ceramic membrane is 0.3 μm, and the running time is 2h.
The drying temperature is 65 ℃ and the drying time is 1h.
Comparative example 2
A technology for preparing sodium carbonate from industrial salt by using a membrane method comprises the following operation steps:
s1: 85g of industrial salt and deionized water with the temperature of 55 ℃ are weighed, stirred and dissolved, and then 20g of NaOH solution with the concentration of 0.08mol/L is added;
s2: adding anti-scaling microspheres with the mass percentage of 0.52 percent of the solution; stirring for 10 minutes at normal temperature, and then filtering the solution by using a ceramic membrane device;
s3: evaporating the filtered filtrate at 85 ℃ for 5 hours, separating the obtained crystal slurry in a centrifuge, and adding 25g of saturated sodium carbonate solution into the centrifuge to wash a filter cake;
s4: and drying the product obtained by centrifugation to obtain the high-purity sodium carbonate.
The pore diameter of the ceramic membrane is 0.3 μm, and the running time is 2h.
The drying temperature is 65 ℃ and the drying time is 1h.
The anti-scaling microsphere is prepared according to the following process steps:
uniformly mixing 5g of tetrabutyl titanate hydrolytic sol and 20g of silane hydrolytic sol, stirring for 2 hours, adding 3g of acrylic acid monomer pre-emulsion and 0.15g of photoinitiator, uniformly stirring, controlling the temperature to 40 ℃ under ultraviolet irradiation, stirring, reacting for 3 hours, centrifuging after the reaction is completed, washing, and drying to obtain the anti-scaling microsphere.
The tetrabutyl titanate hydrolytic sol is prepared by mixing tetrabutyl titanate, acetylacetone and pure water according to the molar ratio of 10:35:0.5 Stirring at 40 ℃ for 1h.
The silane hydrolytic sol is prepared by uniformly mixing methyltrimethoxysilane, acryloxytrimethylsilane, isopropanol and pure water according to a molar ratio of 1:1:2:6, adding 1% hydrochloric acid, and carrying out hydrolysis reaction at 40 ℃ for 60 min.
The acrylic acid monomer pre-emulsion is obtained by uniformly mixing an acrylic acid monomer, sodium dodecyl benzene sulfonate serving as an emulsifier and pure water according to a mass ratio of 1:0.01:10, and then fully stirring and emulsifying.
The acrylic acid monomer is methyl acrylate.
The initiator is bis (2, 4, 6-trimethylbenzoyl) phenylphosphine oxide.
Comparative example 3
A technology for preparing sodium carbonate from industrial salt by using a membrane method comprises the following operation steps:
s1: 85g of industrial salt and deionized water with the temperature of 55 ℃ are weighed, stirred and dissolved, and then 20g of NaOH solution with the concentration of 0.08mol/L is added;
s2: adding anti-scaling microspheres with the mass percentage of 0.52 percent of the solution; stirring for 10 minutes at normal temperature, and then filtering the solution by using a ceramic membrane device;
s3: evaporating the filtered filtrate at 85 ℃ for 5 hours, separating the obtained crystal slurry in a centrifuge, and adding 25g of saturated sodium carbonate solution into the centrifuge to wash a filter cake;
s4: and drying the product obtained by centrifugation to obtain the high-purity sodium carbonate.
The pore diameter of the ceramic membrane is 0.3 μm, and the running time is 2h.
The drying temperature is 65 ℃ and the drying time is 1h.
The anti-scaling microsphere is prepared according to the following process steps:
uniformly mixing 5g of tetrabutyl titanate hydrolytic sol and 20g of silane hydrolytic sol, stirring for 2 hours, then adding 0.25g of rare earth oxide nanocrystalline, stirring for 24 hours, then adding 3g of acrylic acid monomer pre-emulsion, stirring for 3 hours, centrifuging after the reaction is completed, washing and drying to obtain the anti-scaling microsphere.
The tetrabutyl titanate hydrolytic sol is prepared by mixing tetrabutyl titanate, acetylacetone and pure water according to the molar ratio of 10:35:0.5 Stirring at 40 ℃ for 1h.
The silane hydrolytic sol is prepared by uniformly mixing methyltrimethoxysilane, acryloxytrimethylsilane, isopropanol and pure water according to a molar ratio of 1:1:2:6, adding 1% hydrochloric acid, and carrying out hydrolysis reaction at 40 ℃ for 60 min.
The acrylic acid monomer pre-emulsion is obtained by uniformly mixing an acrylic acid monomer, sodium dodecyl benzene sulfonate serving as an emulsifier and pure water according to a mass ratio of 1:0.01:10, and then fully stirring and emulsifying.
The acrylic acid monomer is methyl acrylate.
The rare earth oxide nanocrystalline is obtained by mixing gadolinium oxide nanocrystalline and erbium oxide nanocrystalline according to the mass ratio of 1:0.8.
The sodium carbonate yield, purity, magnesium ion concentration and chloride ion concentration detection results obtained by the above examples and comparative examples are shown in the following table:
the above description is only illustrative of the preferred embodiments of the present invention and is not intended to limit the scope of the present invention, and any alterations and modifications made by those skilled in the art based on the above disclosure shall fall within the scope of the appended claims.
Claims (10)
1. A technology for preparing sodium carbonate from industrial salt by using a membrane method comprises the following operation steps:
s1: weighing 85-100 parts by mass of industrial salt and deionized water at 55-65 ℃, stirring and dissolving, and then adding 20-25 parts by mass of NaOH solution with the concentration of 0.08-0.1 mol/L;
s2: adding anti-scaling microspheres with the mass percentage content of 0.52-2.5 percent into the solution; stirring for 10-30 minutes at normal temperature, and then filtering the solution by using a ceramic membrane device;
s3: evaporating the filtered filtrate at 85-100deg.C for 5-8 hr, separating the obtained crystal slurry with centrifuge, and adding 25-45 parts saturated sodium carbonate solution into the centrifuge to wash filter cake;
s4: and drying the product obtained by centrifugation to obtain the high-purity sodium carbonate.
2. The technology for preparing sodium carbonate from industrial salt by using a membrane method according to claim 1, wherein the technology comprises the following steps: the pore diameter of the ceramic membrane is 0.3-0.8 mu m, and the running time is 2-6h.
3. The technology for preparing sodium carbonate from industrial salt by using a membrane method according to claim 1, wherein the technology comprises the following steps: the drying temperature is 65-80 ℃ and the drying time is 1-4h.
4. The technology for preparing sodium carbonate from industrial salt by using a membrane method according to claim 1, wherein the technology comprises the following steps: the anti-scaling microsphere is prepared according to the following process steps:
according to the parts by weight, uniformly mixing 5-12 parts of butyl titanate hydrolytic sol and 20-32 parts of silane hydrolytic sol, stirring for 2-5 hours, then adding 0.25-0.6 part of rare earth oxide nanocrystalline, stirring for reaction for 24-48 hours, then adding 3-6 parts of acrylic acid monomer pre-emulsion and 0.15-0.38 part of photoinitiator, uniformly stirring, controlling the temperature to 40-60 ℃ under ultraviolet irradiation, stirring for reaction for 3-6 hours, centrifuging after the reaction is completed, washing, and drying to obtain the anti-scaling microspheres.
5. The technology for preparing sodium carbonate from industrial salt by using a membrane method according to claim 4, wherein the technology comprises the following steps: the tetrabutyl titanate hydrolytic sol is prepared by mixing tetrabutyl titanate, acetylacetone and pure water according to the molar ratio of 10:35-40:0.5-1.2, and stirring at 40-60deg.C for 1-3 hr.
6. The technology for preparing sodium carbonate from industrial salt by using a membrane method according to claim 4, wherein the technology comprises the following steps: the silane hydrolytic sol is prepared by uniformly mixing methyltrimethoxysilane, acryloxytrimethylsilane, isopropanol and pure water according to a molar ratio of 1:1:2-6:6-8, adding 1-3% of hydrochloric acid, and carrying out hydrolysis reaction for 60-120min at 40-60 ℃.
7. The technology for preparing sodium carbonate from industrial salt by using a membrane method according to claim 4, wherein the technology comprises the following steps: the acrylic acid monomer pre-emulsion is obtained by uniformly mixing an acrylic acid monomer, sodium dodecyl benzene sulfonate serving as an emulsifier and pure water according to the mass ratio of 1:0.01-0.1:10-15, and then fully stirring and emulsifying.
8. The technology for preparing sodium carbonate from industrial salt by using a membrane method according to claim 4, wherein the technology comprises the following steps: the acrylic acid monomer is methyl acrylate or isopropyl methacrylate or butyl methacrylate.
9. The technology for preparing sodium carbonate from industrial salt by using a membrane method according to claim 4, wherein the technology comprises the following steps: the rare earth oxide nanocrystalline is obtained by mixing gadolinium oxide nanocrystalline and erbium oxide nanocrystalline according to the mass ratio of 1:0.8-1.6.
10. The technology for preparing sodium carbonate from industrial salt by using a membrane method according to claim 4, wherein the technology comprises the following steps: the light initiator is bis (2, 4, 6-trimethylbenzoyl) phenylphosphine oxide or 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone or bisbenzoylphenylphosphine oxide.
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