CN103407970A - Method for preparing sodium percarbonate - Google Patents
Method for preparing sodium percarbonate Download PDFInfo
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- CN103407970A CN103407970A CN2013103328704A CN201310332870A CN103407970A CN 103407970 A CN103407970 A CN 103407970A CN 2013103328704 A CN2013103328704 A CN 2013103328704A CN 201310332870 A CN201310332870 A CN 201310332870A CN 103407970 A CN103407970 A CN 103407970A
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- Prior art keywords
- sodium
- hydrogen peroxide
- sodium percarbonate
- mixing tank
- spc
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- Granted
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- 238000000034 method Methods 0.000 title claims abstract description 36
- VTIIJXUACCWYHX-UHFFFAOYSA-L disodium;carboxylatooxy carbonate Chemical compound [Na+].[Na+].[O-]C(=O)OOC([O-])=O VTIIJXUACCWYHX-UHFFFAOYSA-L 0.000 title claims abstract description 22
- 229940045872 sodium percarbonate Drugs 0.000 title claims abstract description 22
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 73
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 59
- 239000002245 particle Substances 0.000 claims abstract description 31
- 238000007599 discharging Methods 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 22
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000012216 screening Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims description 36
- 239000007921 spray Substances 0.000 claims description 23
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 239000008187 granular material Substances 0.000 claims description 9
- 238000010298 pulverizing process Methods 0.000 claims description 8
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 6
- 239000001488 sodium phosphate Substances 0.000 claims description 5
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 5
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- HQAITFAUVZBHNB-UHFFFAOYSA-N sodium;pentahydrate Chemical compound O.O.O.O.O.[Na] HQAITFAUVZBHNB-UHFFFAOYSA-N 0.000 claims description 4
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 4
- JSYPRLVDJYQMAI-ODZAUARKSA-N (z)-but-2-enedioic acid;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)\C=C/C(O)=O JSYPRLVDJYQMAI-ODZAUARKSA-N 0.000 claims description 3
- 229920002126 Acrylic acid copolymer Polymers 0.000 claims description 3
- 101710194948 Protein phosphatase PhpP Proteins 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 3
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 3
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 claims description 3
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 3
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 3
- 229960004418 trolamine Drugs 0.000 claims description 3
- VPTUPAVOBUEXMZ-UHFFFAOYSA-N (1-hydroxy-2-phosphonoethyl)phosphonic acid Chemical compound OP(=O)(O)C(O)CP(O)(O)=O VPTUPAVOBUEXMZ-UHFFFAOYSA-N 0.000 claims description 2
- CCVYRRGZDBSHFU-UHFFFAOYSA-N (2-hydroxyphenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC=C1O CCVYRRGZDBSHFU-UHFFFAOYSA-N 0.000 claims description 2
- BPSYZMLXRKCSJY-UHFFFAOYSA-N 1,3,2-dioxaphosphepan-2-ium 2-oxide Chemical compound O=[P+]1OCCCCO1 BPSYZMLXRKCSJY-UHFFFAOYSA-N 0.000 claims description 2
- MOMKYJPSVWEWPM-UHFFFAOYSA-N 4-(chloromethyl)-2-(4-methylphenyl)-1,3-thiazole Chemical compound C1=CC(C)=CC=C1C1=NC(CCl)=CS1 MOMKYJPSVWEWPM-UHFFFAOYSA-N 0.000 claims description 2
- JKTORXLUQLQJCM-UHFFFAOYSA-N 4-phosphonobutylphosphonic acid Chemical compound OP(O)(=O)CCCCP(O)(O)=O JKTORXLUQLQJCM-UHFFFAOYSA-N 0.000 claims description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- QILXPCHTWXAUHE-UHFFFAOYSA-N [Na].NCCN Chemical compound [Na].NCCN QILXPCHTWXAUHE-UHFFFAOYSA-N 0.000 claims description 2
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 2
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 2
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 2
- 235000019800 disodium phosphate Nutrition 0.000 claims description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- 238000012423 maintenance Methods 0.000 claims description 2
- 229940045641 monobasic sodium phosphate Drugs 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 235000021317 phosphate Nutrition 0.000 claims description 2
- 150000003016 phosphoric acids Chemical class 0.000 claims description 2
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 229910000160 potassium phosphate Inorganic materials 0.000 claims description 2
- 229940093916 potassium phosphate Drugs 0.000 claims description 2
- 235000011009 potassium phosphates Nutrition 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- 235000019983 sodium metaphosphate Nutrition 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 235000011008 sodium phosphates Nutrition 0.000 claims description 2
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 abstract description 12
- 239000001301 oxygen Substances 0.000 abstract description 12
- 239000013078 crystal Substances 0.000 abstract description 4
- 239000010865 sewage Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 238000005507 spraying Methods 0.000 abstract description 3
- 239000003381 stabilizer Substances 0.000 abstract 1
- 239000013077 target material Substances 0.000 abstract 1
- 235000017550 sodium carbonate Nutrition 0.000 description 16
- 239000000203 mixture Substances 0.000 description 9
- 238000001035 drying Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000000243 solution Substances 0.000 description 5
- 238000007710 freezing Methods 0.000 description 4
- 230000008014 freezing Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000003599 detergent Substances 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000004061 bleaching Methods 0.000 description 2
- MQRJBSHKWOFOGF-UHFFFAOYSA-L disodium;carbonate;hydrate Chemical compound O.[Na+].[Na+].[O-]C([O-])=O MQRJBSHKWOFOGF-UHFFFAOYSA-L 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- WRUGWIBCXHJTDG-UHFFFAOYSA-L magnesium sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Mg+2].[O-]S([O-])(=O)=O WRUGWIBCXHJTDG-UHFFFAOYSA-L 0.000 description 1
- 229940061634 magnesium sulfate heptahydrate Drugs 0.000 description 1
- 230000005405 multipole Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000006072 paste Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- MSLRPWGRFCKNIZ-UHFFFAOYSA-J tetrasodium;hydrogen peroxide;dicarbonate Chemical compound [Na+].[Na+].[Na+].[Na+].OO.OO.OO.[O-]C([O-])=O.[O-]C([O-])=O MSLRPWGRFCKNIZ-UHFFFAOYSA-J 0.000 description 1
- 239000000606 toothpaste Substances 0.000 description 1
- 229940034610 toothpaste Drugs 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- -1 worm conveyor Substances 0.000 description 1
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Abstract
The invention discloses a method for preparing sodium percarbonate, which mainly comprises the following steps: preparing a hydrogen peroxide solution; adding fine sodium percarbonate particles into a mixer with cooling equipment to serve as crystal nucleus; spraying the hydrogen peroxide solution into the mixer, and starting the cooling equipment to keep the system reaction temperature at 20 DEG C to 60 DEG C; adding anhydrous light sodium carbonate and a solid stabilizer into the mixer via transportation equipment; when the particle size of sodium percarbonate products reaches 0.5 mm to 1.2 mm, discharging the products; meanwhile, adjusting the feeding speed and the discharging speed to maintain the constant material in the mixer; screening the discharged sodium carbonate products by virtue of screening equipment, wherein the fine sodium percarbonate products with particle size less than 0.5 mm are returned to the mixer as crystal nucleus in a quantitative manner and the middle target materials with particle size within 0.5 mm and 1.2 mm are dried to be finished products. The method for preparing sodium percarbonate is environmentally friendly, small in equipment investment and simple in technology, produces no sewage, and can prepare the high-quality products with high active oxygen, excellent heat stability and excellent humidity stability.
Description
Technical field
The present invention relates to field of fine chemical, a kind of method for preparing SPC-D particularly, the method is environmentally friendly, and without sewage, facility investment is little, technique is simple, can prepare high-quality product.
Background technology
SPC-D (Sodium Percarbonate) has another name called sodium carbonate peroxide.SPC-D is soluble in water, discharges active oxygen, and the effect that possesses bleaching, sterilization, deoils and wash is widely used as washing composition and the color additive that floats washing powder, also is applied to as in the daily chemical products such as toothpaste, makeup.As new and effective detergent bleach agent, it has odorless, nontoxic, free of contamination characteristics.Owing in water, decomposing the active oxygen produced, has bleaching action, therefore SPC-D shows very strong soil removability, with traditional phosphorus system, boron, is that washing auxiliary detergent is compared, not only strong detergency, and can not destroy ecotope, become one of main washing auxiliary detergent of widespread use in the world at present.
At present, the production method of SPC-D mainly contains two kinds of dry method and wet methods: dry production be by the aqueous solution Direct spraying of hydrogen peroxide to the anhydrous sodium carbonate solid and make the SPC-D crystal; Wet production is to react adding under appropriate stablizer and certain temperature condition with certain density hydrogen peroxide with saturated sodium carbonate solution, then through crystallization, filtration, drying, obtains product.
Patent patent application CN200510100941.3(Guangdong Zhongcheng Chemicals Inc.) a kind of method of preparing sodium carbonate by dry is disclosed.Its method is substantially as follows: add anhydrous solid soda ash in the mixing tank with refrigerating unit, and spray 20%-50% hydrogen peroxide, segmentation regulation and control rate of addition, after reaction finished, the operations such as drying, pulverizing, granulation reached desired product.It is that slurry or paste are difficult to from mixing tank, taking out that the wet feed of this technique is crossed carbon, the product that after taking out, crushed after being dried obtains, and particle is non-spherical, simultaneously the stability of product is not drawn a conclusion yet, and only rests on the lab scale stage.
Russ P RU2245842 C2 provides a kind of technique for preparing SPC-D, first prepares the aqueous sodium carbonate that massfraction is 19.0%-22.5%, for shortening dissolution time, adopts simultaneously ultrasonic technology, can significantly reduce salt sedimentation, extends life cycle.Sodium carbonate solution and hydrogen peroxide (H
2O
2) solution for example adds, in stablizer (sodium sulfate) situation at the same time, reacts in reactor, then enter double-screw mixer, then enter fluid bed dryer.The motor of the motor of mixing tank twin screw and moisture eliminator fan all is equipped with the variable frequency adjustment device, but fine tuning operating parameter whereby, to obtain the product index required.The classifier that dried product introduction is comprised of 2 grades of reciprocating sieves, the screening of middle granularity enters another pneumatic classification device as target product, by (0.1-0.2mm) particle that pressurized air will be thinner, send mixing tank back to through cyclonic separator, namely obtain product after this separates; Volume particle size screening after above-mentioned classification merges with the fine particle screening after pulverizer is pulverized, also by pressurized air, send it back to mixing tank through cyclonic separator.In mixing tank, reactant is along the fine particle surface arrangement that can be used as crystal seed and enter, and wetting its surface, make the fine particle product granularity close in process and constantly increase in wet mixing, in patent, also particularly point out, reactor can move along mixer screw, can change the position that reactant enters mixing tank like this, thereby adjustable product granularity and production capacity, with the optimization of minimum energy consumption implementation procedure.For reactor can be moved along mixing tank, the pipeline that raw material enters reactor consists of flexible metal tube, and mixing tank top is to be covered tightly by some groups of dismountable long 400mm metal sheets, but the movement of complex reaction device provides the reaction mass entrance.The data such as bulk density, active oxygen massfraction, stability (active oxygen rate of loss) of different-grain diameter product in patent, have been provided.Particle diameter is the product of 0.3-1.0mm, and its bulk density is 1.12-1.17g/cm
3, the active oxygen massfraction is 14.25%-14.01%, the active oxygen rate of loss is 3.84%-3.65% (keeping 15h under 65 ℃, 100% humidity).
Also there is the application Patents in the companies such as U.S.'s richness is beautiful in fact simultaneously, Korea S's enlightening is uncommon, Sol dimension, win wound Degussa.Its method is substantially as follows: the anhydrous sodium carbonate particle that passes through to add 74mm-300mm of mentioning in the rich U.S. real US5045296 of the U.S. and US5328721, the hydrogen peroxide of spray 50%-75% is made Sodium Percarbonate Particles, and the product particle of gained is as raw material sodium carbonate size distribution; In U.S. US5851420, put down in writing, add magnesium sulfate heptahydrate in hydrogen peroxide, reaction wherein adds unpurified anhydrous sodium carbonate, hydrogen peroxide sprays in reactor, fluidised bed drying, obtain the particulate state SPC-D, mention simultaneously use-5-20 ℃ of air cooling, every cube of reactor air flow is 0.5-80m3/min.The method comparing class of a CN200510100941.3 preparing sodium carbonate by dry of the Germany Suo Weiyingte CN97180679.9 of company of AUX and Guangdong Zhongcheng Chemicals Inc. seemingly, in CN97180679.9, should be mentioned that by monohydrate sodium carbonate and set out, with the 55%-60% hydrogen peroxide solution, through double nozzle, carry out powerful mixing in mixing tank, later stage, the material that then will lump obtained 550-1100um by pulverizing and sieving by adding or do not add the lubricant briquetting.Korea S's enlightening is uncommon is mainly that the spray hydrogen peroxide, after certain content, is transferred to secondary spraying hydrogen peroxide in fluidized-bed and obtained the SPC-D product in double cone mixer.Other companies are also limit spray hydrogen peroxide in fluidized-bed substantially, the limit drying.Its raw material has two kinds of Soda Ash Light 99.2min. or Soda Ash Danses.
In sum, Russ P is by after the sodium carbonate wiring solution-forming, carries out liquid-liquid reactions; The rich U.S. of the U.S. is real is to add the anhydrous sodium carbonate particle, then sprays in the above hydrogen peroxide solution and reacts; Germany Solvay is from monohydrate sodium carbonate, and spray adds lubricant briquetting, flour, granulation after hydrogen peroxide and obtains SPC-D in mixing tank.All the other carry out the SPC-D dry method is substantially all fluidized-bed spray, drying-granulating; Existence is strict to equipment, and dust is larger, and temperature is controlled and with great difficulty do not caused hydrogen peroxide to consume the problems such as high.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing SPC-D of novelty, environmentally friendly, without sewage, facility investment is little, technique is simple, can prepare high-quality product.
A kind of method for preparing SPC-D, is characterized in that, mainly comprises the following steps:
A. prepare hydrogen peroxide solution: in hydrogen peroxide solution, add stablizer, stir, be made into the solution that the hydrogen peroxide mass concentration is 27.5%-70%;
B. in the mixing tank with cooling apparatus, adding particle diameter is that 0.15 mm-0.5mm, moisture content are that the sodium percarbonate granules of 0-20% is as nucleus; In mixing tank, spray hydrogen peroxide solution, open cooling apparatus, the maintenance system temperature of reaction is 20 ℃-60 ℃; The anhydrous light sodium carbonate and the Pickering agent that by particle diameter, are 1-150 μ m add in mixing tank by transmission equipment, and it is 1: 3.05 ~ 4.72 that the flow by regulating hydrogen peroxide and light sodium carbonate transfer rate are controlled the two weight ratio;
C. when the SPC-D product cut size reaches 0.5mm-1.2mm, discharging; Regulating simultaneously input speed and discharging speed, to maintain the mixing tank material constant;
D. the sodium carbonate product of discharging is sieved with screening plant, get the above material of 1.2mm by pulverizing, after screening as finished product, the following tiny SPC-D of particle diameter 0.5mm is quantitatively returned in mixing tank as nucleus, and the intermediate objective material of 0.5mm-1.2mm is dried to obtain finished product.
Innovation point of the present invention is to make soda ash by contacting, carry out the moment reaction with hydrogen peroxide on the one hand, by mixing equipment, impel the moment resultant to be wrapped on the SPC-D nucleus in mixing tank simultaneously, take into account chemical reaction and mechanical force and produce evenly, the Sodium Percarbonate Particles of fine and close, quality better.
The present invention is mainly by adding the sodium percarbonate granules bottoming as nucleus, add the anhydrous Soda Ash Light 99.2min. of certain order number on one side, spray hydrogen peroxide solution on one side, continuous feeding and discharging, pass into Cryogenic air and take away the solution heat of reaction heat and soda ash, simultaneously the tiny SPC-D nucleus after discharging is quantitatively returned in mixed system to secondary response again, so repeatedly reach the purpose of continuous production graininess SPC-D product.
Further; stablizer described in steps A is selected from hydroxy ethylene diphosphonic acid, Amino Trimethylene Phosphonic Acid, sodium ethylenediamine tetramethylenephosphonate, 2-phosphonic acids butane-1; one or more in 2,4-tricarboxylic acid, 2-HPAA, maleic acid-acrylic acid copolymer, sodium polyacrylate, trolamine, magnesium chloride, sal epsom or EDTA.
In steps A, the hydrogen peroxide mass concentration is preferably 50-60%.
Sodium percarbonate granules particle diameter as nucleus in step B is preferably 0.3-0.5mm, and moisture content is preferably 0-10%.
In step B, anhydrous light sodium carbonate particle diameter is preferably 40-80 μ m.
Pickering agent described in step B is selected from the silicate such as metasilicate pentahydrate sodium, Sodium hexametaphosphate 99; Phosphoric acid salt is one or more in SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate dibasic, sodium phosphate, trisodium phosphate, sodium-metaphosphate, tripoly phosphate sodium STPP, potassium primary phosphate, dipotassium hydrogen phosphate or potassiumphosphate.
In step B, temperature of reaction is preferably 25 ℃-35 ℃.
The described mixing tank of step B is cone mixer or mixing screw.The inventive method is reacted by contacting with hydrogen peroxide by soda ash on the one hand, by mixing equipment, impels the moment resultant to be wrapped on the SPC-D nucleus simultaneously, less demanding to equipment, however the particle that is broken to type can be applicable to.
The described cooling apparatus of step B comprises pneupress system equipment, gas blower, air cooler, and other the several kind equipment that can lower the temperature and take away the system heat all can be used.Because sodium carbonate exothermic dissolution and exothermic heat of reaction need to be removed the waste heat of system in time, reduce the consumption of hydrogen peroxide, therefore for the equipment that the low temperature cold air source can be provided, can reach cooling-down effect.But the transmission equipment of soda ash and Pickering agent can be the equipment of the transferring raw materials such as worm conveyor, powder pneumatic handling equipment, conveying belt.The dioxygen water pump preferably is equipped with frequency transformer, regulates the flow of hydrogen peroxide solution with this.
The particle process coarse reduction that 1.2mm in step D is above, get tiny SPC-D as in nucleus material Returning reacting system.
The present invention prepares the method for SPC-D, environmentally friendly, and without sewage, facility investment is little, technique is simple, can prepare high-quality product, and Product Activity oxygen is high, thermostability and wet good stability.
The accompanying drawing explanation
Fig. 1 is the equipment schematic diagram that the present invention prepares SPC-D.
Embodiment
Embodiment 1
By the 10kg particle diameter, be that the 0.5mm small sodium percarbonate particles is added in the 50L double-cone mixer, add simultaneously 0.2kg Pickering agent sal epsom, take the 50kg hydrogen peroxide solution (with H
2O
2Meter 50.1%), and add 0.5kgHEDP and sodium salt solution thereof, be uniformly mixed.Add in addition the 0.6kg metasilicate pentahydrate sodium in 80um 56kg Soda Ash Light 99.2min., mix.In double-cone mixer, spray the hydrogen peroxide solution prepared, open freezing recirculated water and the cooling of multipole gas blower, when hydrogen peroxide sprays 0.8kg, Yi Bian spray hydrogen peroxide solution, Yi Bian add the Soda Ash Light 99.2min. mixture.When the SPC-D product cut size reaches 0.5mm-1.2mm, discharging.According to the material particular diameter in still, add simultaneously the sodium percarbonate granules control product cut size of 0.3mm, the 1.2mm of discharging is above returns to the material below 0.5mm to mixing wherein after pulverizing, as long as continuous time, material is prepared burden according to above continuation, so repeatedly, continuous feeding and discharging, drying.Product Activity oxygen 13.2%, thermostability 85%(90 ℃, 24h), wet stability 64%, median size 810um.
Embodiment 2
15kg 0.4mm small sodium percarbonate particles is added in the 50L double-cone mixer, adds simultaneously 0.15kg Pickering agent sal epsom, take the 50kg hydrogen peroxide solution (with H
2O
2Meter 60.1%), and add 0.45kg Amino Trimethylene Phosphonic Acid and sodium salt solution thereof, be uniformly mixed.Add in addition the 0.4kg Sodium hexametaphosphate 99 in 80um 60kg Soda Ash Light 99.2min., mix.In single cone mixing machine, spray the hydrogen peroxide solution prepared, open freezing recirculated water and the cooling of pressurized air unit, when hydrogen peroxide sprays 0.45kg, Yi Bian spray hydrogen peroxide solution, Yi Bian add the Soda Ash Light 99.2min. mixture.When the SPC-D product cut size reaches 0.5mm-1.2mm, discharging.According to the material particular diameter in still, add simultaneously the sodium percarbonate granules control product cut size of 0.36mm, the 1.2mm of discharging is above returns to the material below 0.5mm to mixing wherein after pulverizing, as long as continuous time, material is prepared burden according to above continuation, so repeatedly, continuous feeding and discharging, drying.Product Activity oxygen 14.2%, thermostability 80%(90 ℃, 24h), wet stability 68%, median size 840um.
Embodiment 3
8kg 0.5mm small sodium percarbonate particles is added in the 50L double-cone mixer, adds simultaneously 0.4kg Pickering agent sal epsom, take the 100kg hydrogen peroxide solution (with H
2O
2Meter 55%), and add the 1.2kg maleic acid-acrylic acid copolymer, be uniformly mixed.Add in addition 0.9kg metasilicate pentahydrate sodium and 0.5kg tripoly phosphate sodium STPP in 80um 80kg Soda Ash Light 99.2min., mix.In double-cone mixer, spray the hydrogen peroxide solution prepared, open freezing recirculated water and multistage blowers cooling, when hydrogen peroxide sprays 0.24kg, Yi Bian spray hydrogen peroxide solution, Yi Bian add the Soda Ash Light 99.2min. mixture.When the SPC-D product cut size reaches 0.5mm-1.2mm, discharging.According to the material particular diameter in still, add simultaneously the sodium percarbonate granules control product cut size of 0.3mm, the 1.2mm of discharging is above returns to the material below 0.5mm to mixing wherein after pulverizing, as long as continuous time, material is prepared burden according to above continuation, so repeatedly, continuous feeding and discharging, drying.Product Activity oxygen 13.7%, thermostability 84%(90 ℃, 24h), wet stability 72%, median size 750um.
Embodiment 4
10kg 0.5mm small sodium percarbonate particles is added in the 50L double-cone mixer, adds simultaneously 1.2kg Pickering agent sal epsom, take the 100kg hydrogen peroxide solution (with H
2O
2Meter 55%), and add the 1.2kg trolamine, be uniformly mixed.Add in addition the 1.9kg trisodium phosphate in 80um 80kg Soda Ash Light 99.2min., mix.In the simple helix mixing machine, spray the hydrogen peroxide solution prepared, open freezing recirculated water and multistage blowers cooling, when hydrogen peroxide sprays 0.3kg, Yi Bian spray hydrogen peroxide solution, Yi Bian add the Soda Ash Light 99.2min. mixture.When the SPC-D product cut size reaches 0.5mm-1.2mm, discharging.According to the material particular diameter in still, add simultaneously the sodium percarbonate granules control product cut size of 0.3mm, the 1.2mm of discharging is above returns to the material below 0.5mm to mixing wherein after pulverizing, as long as continuous time, material is prepared burden according to above continuation, so repeatedly, continuous feeding and discharging, drying.Product Activity oxygen 14.0%, thermostability 80%(90 ℃, 24h), wet stability 67%, median size 890um.
Claims (10)
1. a method for preparing SPC-D, is characterized in that, mainly comprises the following steps:
A. prepare hydrogen peroxide solution: in hydrogen peroxide solution, add stablizer, stir, be made into the solution that the hydrogen peroxide mass concentration is 27.5%-70%;
B. in the mixing tank with cooling apparatus, adding particle diameter is that 0.15 mm-0.5mm, moisture content are that the sodium percarbonate granules of 0-20% is as nucleus; In mixing tank, spray hydrogen peroxide solution, open cooling apparatus, the maintenance system temperature of reaction is 20 ℃-60 ℃; The anhydrous light sodium carbonate and the Pickering agent that by particle diameter, are 1-150 μ m add in mixing tank by transmission equipment, and it is 1: 3.05 ~ 4.72 that the flow by regulating hydrogen peroxide and light sodium carbonate transfer rate are controlled the two weight ratio;
C. when the SPC-D product cut size reaches 0.5mm-1.2mm, discharging; Regulating simultaneously input speed and discharging speed, to maintain the mixing tank material constant;
D. the sodium carbonate product of discharging is sieved with screening plant, get the above material of 1.2mm by pulverizing, after screening as finished product, the following tiny SPC-D of particle diameter 0.5mm is quantitatively returned in mixing tank as nucleus, and the intermediate objective material of 0.5mm-1.2mm is dried to obtain finished product.
2. method according to claim 1; it is characterized in that; stablizer described in steps A is selected from hydroxy ethylene diphosphonic acid, Amino Trimethylene Phosphonic Acid, sodium ethylenediamine tetramethylenephosphonate, 2-phosphonic acids butane-1; one or more in 2,4-tricarboxylic acid, 2-HPAA, maleic acid-acrylic acid copolymer, sodium polyacrylate, trolamine, magnesium chloride, sal epsom or EDTA.
3. method according to claim 1, is characterized in that, in steps A, the hydrogen peroxide mass concentration is 50-60%.
4. method according to claim 1, is characterized in that, the sodium percarbonate granules particle diameter as nucleus in step B is 0.3-0.5mm, and moisture content is 0-10%.
5. method according to claim 1, is characterized in that, in step B, anhydrous light sodium carbonate particle diameter is 40-80 μ m.
6. method according to claim 1, is characterized in that, the Pickering agent described in step B is selected from the silicate such as metasilicate pentahydrate sodium, Sodium hexametaphosphate 99; Phosphoric acid salt is one or more in SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate dibasic, sodium phosphate, trisodium phosphate, sodium-metaphosphate, tripoly phosphate sodium STPP, potassium primary phosphate, dipotassium hydrogen phosphate or potassiumphosphate.
7. method according to claim 1, is characterized in that, in step B, temperature of reaction is 25 ℃-35 ℃.
8. method according to claim 1, is characterized in that, the described mixing tank of step B is cone mixer or mixing screw.
9. method according to claim 1, is characterized in that, the described cooling apparatus of step B comprises pneupress system equipment, gas blower, air cooler.
10. method according to claim 1, is characterized in that, the particle process coarse reduction that the 1.2mm in step D is above, get tiny SPC-D as in nucleus material Returning reacting system.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104012458A (en) * | 2014-05-07 | 2014-09-03 | 浙江金科过氧化物股份有限公司 | Method for preparing oxygen producer through byproduct large-particle sodium percarbonate |
| CN104591098A (en) * | 2014-12-31 | 2015-05-06 | 浙江金科过氧化物股份有限公司 | Method for preparing novel sodium percarbonate |
| CN108483406A (en) * | 2018-04-19 | 2018-09-04 | 周大凯 | A kind of method that nanometer highly reactive form of oxygen stable sodium percarbonate is prepared under room temperature |
| CN108726486A (en) * | 2018-07-12 | 2018-11-02 | 绍兴上虞洁华化工有限公司 | The continuous preparation method of SODIUM PERCARBONATE |
| CN110129773A (en) * | 2019-06-19 | 2019-08-16 | 宁波中科纬诚新材料科技有限公司 | A kind of method of chemical nickeling ageing liquid circular regeneration |
| CN111285334A (en) * | 2018-12-10 | 2020-06-16 | 天津大学 | Sodium percarbonate having a compact spherical structure and process for its preparation |
| CN111517287A (en) * | 2020-06-16 | 2020-08-11 | 中国水产科学研究院黄海水产研究所 | Production method of sodium percarbonate for aquaculture, product and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104012458A (en) * | 2014-05-07 | 2014-09-03 | 浙江金科过氧化物股份有限公司 | Method for preparing oxygen producer through byproduct large-particle sodium percarbonate |
| CN104591098A (en) * | 2014-12-31 | 2015-05-06 | 浙江金科过氧化物股份有限公司 | Method for preparing novel sodium percarbonate |
| CN108483406A (en) * | 2018-04-19 | 2018-09-04 | 周大凯 | A kind of method that nanometer highly reactive form of oxygen stable sodium percarbonate is prepared under room temperature |
| CN108726486A (en) * | 2018-07-12 | 2018-11-02 | 绍兴上虞洁华化工有限公司 | The continuous preparation method of SODIUM PERCARBONATE |
| CN111285334A (en) * | 2018-12-10 | 2020-06-16 | 天津大学 | Sodium percarbonate having a compact spherical structure and process for its preparation |
| CN110129773A (en) * | 2019-06-19 | 2019-08-16 | 宁波中科纬诚新材料科技有限公司 | A kind of method of chemical nickeling ageing liquid circular regeneration |
| CN111517287A (en) * | 2020-06-16 | 2020-08-11 | 中国水产科学研究院黄海水产研究所 | Production method of sodium percarbonate for aquaculture, product and application thereof |
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