CN101270232B - Method for preparing particle type coating sodium percarbonate - Google Patents
Method for preparing particle type coating sodium percarbonate Download PDFInfo
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- CN101270232B CN101270232B CN200810060393XA CN200810060393A CN101270232B CN 101270232 B CN101270232 B CN 101270232B CN 200810060393X A CN200810060393X A CN 200810060393XA CN 200810060393 A CN200810060393 A CN 200810060393A CN 101270232 B CN101270232 B CN 101270232B
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- Prior art keywords
- sodium
- sodium percarbonate
- massfraction
- stability
- soda ash
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- 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 24
- 229940045872 sodium percarbonate Drugs 0.000 title claims abstract description 24
- 239000002245 particle Substances 0.000 title claims description 24
- 239000011248 coating agent Substances 0.000 title claims description 21
- 238000000576 coating method Methods 0.000 title claims description 20
- 238000000034 method Methods 0.000 title abstract description 23
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 46
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 239000003381 stabilizer Substances 0.000 claims abstract description 10
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- 235000017550 sodium carbonate Nutrition 0.000 claims description 22
- 239000012452 mother liquor Substances 0.000 claims description 15
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 8
- 239000011343 solid material Substances 0.000 claims description 8
- 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 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- 235000019353 potassium silicate Nutrition 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 6
- 229940120146 EDTMP Drugs 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000007791 liquid phase Substances 0.000 claims description 5
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 5
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 5
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 claims description 4
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 4
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 4
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 4
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 4
- 229940038773 trisodium citrate Drugs 0.000 claims description 4
- -1 Natvosol Chemical compound 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims description 2
- 101710194948 Protein phosphatase PhpP Proteins 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- 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 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 2
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical group [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 239000007921 spray Substances 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 abstract 1
- 239000003642 reactive oxygen metabolite Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 25
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 12
- 239000001301 oxygen Substances 0.000 description 12
- 229910052760 oxygen Inorganic materials 0.000 description 12
- 230000000694 effects Effects 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 4
- 239000007844 bleaching agent Substances 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000002808 molecular sieve Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 3
- 239000001488 sodium phosphate Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 3
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 3
- 235000019801 trisodium phosphate Nutrition 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- HATLBMTXXWWFGW-UHFFFAOYSA-N C1(=CC=CC=C1)[Na].CCCCCCCCCCCC Chemical compound C1(=CC=CC=C1)[Na].CCCCCCCCCCCC HATLBMTXXWWFGW-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229920002401 polyacrylamide Polymers 0.000 description 2
- YKLJGMBLPUQQOI-UHFFFAOYSA-M sodium;oxidooxy(oxo)borane Chemical compound [Na+].[O-]OB=O YKLJGMBLPUQQOI-UHFFFAOYSA-M 0.000 description 2
- 239000003206 sterilizing agent Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical group [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical class OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910000318 alkali metal phosphate Inorganic materials 0.000 description 1
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 1
- 229910052936 alkali metal sulfate Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000005452 food preservative Substances 0.000 description 1
- 235000019249 food preservative Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000002762 monocarboxylic acid derivatives Chemical group 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004076 pulp bleaching Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000725 suspension Substances 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
- 239000004753 textile Substances 0.000 description 1
- 230000002110 toxicologic effect Effects 0.000 description 1
- 231100000027 toxicology Toxicity 0.000 description 1
- 239000000984 vat dye Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Abstract
The invention discloses a preparation method of granular film coated sodium percarbonate, which solves the problem of the quite low stability of the prior products. In the invention, hydrogen peroxide and sodium carbonate are used as raw materials, an appropriate stabilizer and process parameters are selected to synthesize the granular type film coated sodium percarbonate product, and the raw materials are treated by the steps of dissolution, reaction, centrifugation, fluid bed spray liquid pocket, drying, etc. to prepare the high-stability granular type film coated sodium percarbonate; the bulk density of the granular type film coated sodium percarbonate prepared by the method of the invention is 750 to 1150kg/m3, the grain size is 0.8 to 1.4mm, the content of reactive oxygen species is 13.1 percent to 13.6 percent; the moisture stability is higher than 70 percent and the thermal stability is higher than 90 percent; the product is widely applicable in daily chemical, organic synthesis and other industrial fields.
Description
Technical field
The present invention relates to field of fine chemical, particularly a kind of preparation method of high stability particle type coating sodium percarbonate and wet method packaging technique.
Background technology
SPC-D (sodium percarbonate) claim sodium carbonate peroxide, chemical general formula 2Na again
2CO
33H
2O
2, relative molecular mass is 314.0, theoretical active o content is 15.28%.Envelope type SPC-D (coated sodium percarbonate) is to be matrix with the granule type SPC-D, superscribes one deck stablizer outside, to improve product stability.
SPC-D also is widely used in aspects such as washing, weaving, medical treatment, papermaking, plating except that as the strong oxidizer, because the active o content of SPC-D is higher, is commonly used for SYNTHETIC OPTICAL WHITNER, sterilant, sterilizing agent and food preservative etc.Utilize SPC-D under catalyst action, can discharge the characteristics of oxygen, also used as the new chemical oxygen source of first aid with oxygen.
SPC-D is compared with early stage peroxide bleaching agents such as chlorine bleaching agent and Sodium peroxoborate when the SYNTHETIC OPTICAL WHITNER, does not have the irritating smell of chlorine bleaching agent; Moiety is to environment and human body toxicological harmless effect, and the low temperature active height, thereby is widely used as SYNTHETIC OPTICAL WHITNER, dyeing and finishing agent, the dry chemicking agent of textile industry, and industry, family's purificant are used as the association with pulp bleaching agent in the paper industry.In addition, it also is used as the developer of vat dyes, the sterilizing agent of food tableware, metal conditioner etc.
SPC-D does not contain harmful boron as the oxygenant in the washing composition, helps reducing the pollution of environment, therefore is subjected to the popular welcome of countries in the world.
SPC-D is unstable in a humid environment, decompose easily and discharge active oxygen, for waiting time that improves product and the purposes that enlarges product, need indexs such as preparation good stability, active o content and solvability to meet the SPC-D product of customer requirements, the various countries scientific research personnel has carried out a large amount of research from all respects such as synthesis technique, reaction conditions, stablizer selections for this reason and has explored, obtained certain achievement, but the stability that up to the present, how further to improve SPC-D remains the biggest problem that domestic and international scientific and technical personnel face jointly.
ZL93115283.6 (notification number CN1031254C) discloses a kind of method of stable sodium percarbonate, what this method obtained is Powdered SPC-D, and stability is relatively poor relatively, and the reaction times in the method is oversize, hydrogen peroxide concentration is low, and industrial application value is not high.
CN1435449A discloses a kind of method that improves package stability, the gradation in vibrated fluidized bed of this method sprays into the stablizer aqueous solution, process is more loaded down with trivial details, and according to patent specification, not having clear and definite product stability is wet stability or thermostability index, and at detergent industry, the stability under the super-humid conditions has prior meaning than thermostability.
GB174891 discloses a kind of in order to improve storage stability water glass solution being sprayed on the chemical combination that contains active oxygen and the method for subsequent drying.Be on the sodium percarbonate granules that crystallization obtains, to apply enough silicate and make SPC-D stable in the DE-OS2652776 disclosed method.But at detergent industry, if SPC-D mesosilicic acid salts contg is too high, easy and calcium ions and magnesium ions forms insoluble substance, is unfavorable for improving washing effect.
The stable method of a kind of particulate state SPC-D is proposed among DE-OS2417572 and the DE-PS2622610, with yellow soda ash or/and sodium sulfate and water glass are coating, keep 30-80 ℃ of fluidized-bed temperature spray to coated material on the particle SPC-D before high product stability.
DE-PS2800916, DE-OS3321082, DE-PS2651442, DE-PS2810379 proposes the salt action lapping with boracic, but because boron has certain disadvantageous effect to environment, so more and more enterprises tends to not use the compound of boracic in washing composition.
CN1369528A is a coating agent with alkali metal phosphate, alkali metal sulfates and alkalimetal silicate, repeatedly applies, and has obtained wet stability greater than 60% SPC-D product.
CN1569971A proposes to make the suspension that concentration is 20-30% with membrane-forming agent, tensio-active agent, vitriol, has made wet preferably stable product.
WO 96/06801 has described the sodium percarbonate granules of the coating with the stability improved, and it is by the nuclear of sodium percarbonate granules, comprises the undercoat of vitriol or silicate and comprise the compound (B) in the salt that is selected from monocarboxylic acid with 4 or more carbon atoms and di-carboxylic acid and be selected from the external coating (EC) of the compound (C) in sulphonated oil, alpha-olefin sulfonic acid and monoalkyl and the dialkyl sulfosuccinates synthetic.Given example explanation in the specification sheets, the existence of compound (B) is necessary for reaching enough stability in storagies, an inclusion compound (C) in external coating (EC) and do not contain the less stable of compound (B).
JP-A06-263434 has described a kind of method that improves SPC-D stability.Increase particulate stability by adding a kind of tensio-active agent.
The SPC-D product of selling on the comprehensive document of publishing both at home and abroad and patent of invention and the market can be recognized, because SPC-D low temperature active height, dissolution rate is fast, be higher than 70% SPC-D if can prepare wet stability, just can replace the original Sodium peroxoborate that uses in the washing composition, but at present in the production method of the stable sodium percarbonate of large-scale commercial production, production cost is often than higher, technology is more complicated also, and wet stability is higher than SPC-D product very difficult acquisition on market of 70%.
Summary of the invention
The object of the present invention is to provide a kind of particle type coating sodium percarbonate, particularly a kind of preparation method of high stability particle type coating sodium percarbonate, this method has easy and simple to handle, the advantage that production cost is low, sintetics yield height, the wet stability and the thermostability height of the particle type coating sodium percarbonate that obtains by this method, and be successfully applied to industrial practice.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of particle type coating sodium percarbonate is characterized in that may further comprise the steps:
A. yellow soda ash, sodium-chlor, internal stabilizer are under agitation added formation yellow soda ash slip in the mother liquor that contains hydrogen peroxide 0.5%～1.0% (massfraction), yellow soda ash 6%～16% (massfraction), sodium-chlor 10%～20% (massfraction) by 100: 14～25: 0.5～5 mass ratio, temperature remains on 30～60 ℃;
B. configuration concentration is the hydrogen peroxide solution of 35% (massfraction), adds 1～4% (massfraction) stablizer;
C. the throughput ratio of controlling yellow soda ash slip and hydrogen peroxide solution is 3: 1 (mass ratio), in the reactor of input tape agitator and cooling jacket;
D. controlling synthesis reaction temperature is 5～30 ℃, and the reaction times is 1～1.5 hour;
E. reaction is finished, and with the reaction product centrifugation, liquid phase is through filter press, the mother liquor reuse;
F. solid materials is removed surperficial moisture content through 80～120 ℃ of heat bakings, carries out the hydrojet dressing at fluidized-bed, gets particle type coating sodium percarbonate.
Further, in the preparation process of SPC-D,, in step c, in reactor, add the SPC-D nucleus for granularity is regulated and control.The raw material of input can be reacted at the nucleus particle surface, and slowly grow up, and make reaction system keep clarification, reduced the quantity of particulate product to desired particle size.
Internal stabilizer among the step a of the present invention comprises tripoly phosphate sodium STPP, Trisodium Citrate, Starso, one or more in magnesium chloride or the sal epsom.
Stablizer among the step b comprises one or more in ethylene diamine tetra methylene phosphonic acid, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, EDTA, sodium polyacrylate or the polyamide solution.
Further, comprise water glass (Na in the hydrojet that dressing uses among the step f
2SiO
3), one or more outer stabilizers in sodium stearate, Natvosol, Sodium dodecylbenzene sulfonate, the sodium laurylsulfonate.
Using the granularity of the particle type coating sodium percarbonate of the inventive method preparation is 0.3～1.4mm, and active o content is 13.1～13.6%, and wet stability is greater than 70%, and thermostability is greater than 90%.Can be widely used in having better storage stability in the daily cleaning products such as washing powder, SYNTHETIC OPTICAL WHITNER, solve the too high problem of currently available products density.The inventive method is a raw material with hydrogen peroxide, yellow soda ash, selects suitable stablizer and suitable processing parameter for use, and is easy and simple to handle, sintetics yield height; And the reusable edible mother liquor helps protecting environment in process of production, has reduced production cost.
Embodiment
Embodiment 1
Preparation mother liquor (800kg): hydrogen peroxide 4kg, yellow soda ash 80kg, sodium-chlor 160kg, water 556kg is stirred to whole dissolvings.
Industrial sodium carbonate 300kg and 6kg Starso, 4kg trisodium phosphate, 2kg EDTA, 70kg sodium-chlor are added to formation yellow soda ash slip in the mother liquor that configures, and temperature remains on 30～60 ℃.
Configuration concentration is the hydrogen peroxide solution 380kg of 35% (massfraction), adds the mixed stabilizer (mass ratio 1: 1: 1) of 12kg ethylene diamine tetra methylene phosphonic acid, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid and EDTA, 1kg sodium polyacrylate and 1kg polyacrylamide.
Add the 100kg mother liquor in the reactor of band cooling jacket and particle diameter is the SPC-D nucleus 5kg of 0.05mm～0.1mm, start agitator motor.The throughput ratio of control yellow soda ash slip and hydrogen peroxide mixed solution is 3: 1 (mass ratio), in yellow soda ash slip and hydrogen peroxide input reactor.
150 rev/mins of control reactor mixing speed, 15～30 ℃ of temperature of reaction, 1.5 hours reaction times.
Reaction finishes, with tripod pendulum type batch centrifugal reaction mass is carried out centrifugal, the mother liquor reuse that liquid phase is reacted as next still after sheet frame tooth filter.
Separating obtained solid materials (wet product) is removed surface-moisture through the baking of vibrated fluidized bed heat, and heat baking temperature is controlled at 80～120 ℃, gets the product that granularity is 0.5～1.4mm, and the fluidized-bed of delivering to subsequent processing carries out the hydrojet dressing.
The prescription of coating liquid is: water 1000kg, water glass (Na
2SiO
3) 50kg, sal epsom 50kg, Natvosol 50kg, sodium laurylsulfonate 50kg, sodium sulfate 100kg is stirred to solid materials and all dissolves, and is injected in the fluidized-bed with pump, and flow is 500kg/h.
The active o content of the coated particle SPC-D that obtains is 13.4%, and under 32 ℃ and 80% relative humidity condition, mixing the remaining activity oxygen level of placing after 48 hours with the 4A molecular sieve of 1: 1 (mass ratio) is 75% of original content.After 100 ℃ were placed 2 hours, the remaining activity oxygen level was 97% of an original content.Under 15 ℃ of conditions, particle dissolution time in water is 2.3 minutes.
Embodiment 2
Industrial sodium carbonate 300kg and 3kg Starso, 4kg trisodium phosphate, 2kg EDTA, 3kg sal epsom, 3kg Trisodium Citrate and 60kg sodium-chlor are added in the reuse mother liquor of specific embodiment 1 and form the yellow soda ash slip, temperature remains on 30～60 ℃.
Configuration concentration is the hydrogen peroxide solution 350kg of 35% (massfraction), adds the mixed stabilizer (mass ratio 1: 4: 1) of 23kg ethylene diamine tetra methylene phosphonic acid, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid and EDTA, the 10kg sodium polyacrylate.
Add the 100kg mother liquor in the reactor of band cooling jacket and particle diameter is the SPC-D nucleus 5kg of 0.05mm～0.1mm, start agitator motor.The throughput ratio of control yellow soda ash slip and hydrogen peroxide is 3: 1 (mass ratio), in yellow soda ash slip and hydrogen peroxide input reactor.
200 rev/mins of control reactor mixing speed, 15～20 ℃ of temperature of reaction, 1.5 hours reaction times.
Reaction finishes, with tripod pendulum type batch centrifugal reaction mass is carried out centrifugal, liquid phase after filter press as the mother liquor reuse of next still reaction.
Separating obtained solid materials (wet product) is removed surface-moisture through the baking of vibrated fluidized bed heat, and heat baking temperature is controlled at 80～120 ℃, gets the product that granularity is 0.5～1.4mm, and the fluidized-bed of delivering to subsequent processing carries out the hydrojet dressing.
The prescription of coating liquid is: water 1000kg, 50kg water glass (Na
2SiO
3), 50kg sal epsom, 100kg dodecane phenyl sodium sulfonate, sodium sulfate 100kg is stirred to solid materials and all dissolves, and is injected in the fluidized-bed with pump, and flow is 500kg/h.
Obtaining the particulate product active o content is 13.5%, and under 32 ℃ and 80% relative humidity condition, mixing the remaining activity oxygen level of placing after 48 hours with the 4A molecular sieve of 1: 1 (mass ratio) is 70% of original content.After 100 ℃ were placed 2 hours, the remaining activity oxygen level was 95% of an original content.Under 15 ℃ of conditions, particle dissolution time in water is 3.4 minutes.
Embodiment 3
Industrial sodium carbonate 300kg and 3kg Starso, 4kg trisodium phosphate, 3kg Trisodium Citrate and 80kg sodium-chlor are added in the reuse mother liquor of specific embodiment 2 and form pulpous state, temperature remains on 30～60 ℃.
Configuration concentration is the hydrogen peroxide solution 350kg of 35% (massfraction), adds the mixed stabilizer (mass ratio 1: 2) of 15kg ethylene diamine tetra methylene phosphonic acid and EDTA, the mixture of 5kg polyacrylamide and sodium polyacrylate (mass ratio 1: 0.5).
Add the 100kg mother liquor in the reactor of band cooling jacket and particle diameter is the SPC-D nucleus 5kg of 0.05mm～0.1mm, start agitator motor.The throughput ratio of control yellow soda ash slip and hydrogen peroxide is 3: 1 (mass ratio), in yellow soda ash slip and hydrogen peroxide input reactor.
150 rev/mins of control reactor mixing speed, 15～30 ℃ of temperature of reaction, 0.5 hour reaction times.
Reaction finishes, with tripod pendulum type batch centrifugal reaction mass is carried out centrifugal, liquid phase after filter press as the mother liquor reuse of next still reaction.
Separating obtained solid materials is removed surface-moisture through the baking of vibrated fluidized bed heat, and heat baking temperature is controlled at 80～120 ℃, gets the product that granularity is 0.5～1.4mm, and the fluidized-bed of delivering to subsequent processing carries out the hydrojet dressing.
The prescription of coating liquid is: water 1000kg, 50kg water glass (Na
2SiO
3), 50kg sal epsom, 50kg dodecane phenyl sodium sulfonate, the 50kg sodium laurylsulfonate, sodium sulfate 100kg is stirred to solid materials and all dissolves, and is injected in the fluidized-bed with pump, and flow is 500kg/h.
The active o content of the coated particle SPC-D that obtains is 13.2%, and under 32 ℃ and 80% relative humidity condition, mixing the remaining activity oxygen level of placing after 48 hours with the 4A molecular sieve of 1: 1 (mass ratio) is 78% of original content.After 100 ℃ were placed 2 hours, the remaining activity oxygen level was 97% of an original content.Under 15 ℃ of conditions, particle dissolution time in water is 2.8 minutes.
The particle type coating sodium percarbonate with low pile density product that obtains according to the present invention and the performance index of domestic and international product of the same type compare:
The contrast of table 1 high stability SPC-D product and similar products at home and abroad index
| Project | The SPC-D that obtains according to the inventive method | Commercially available | Japan |
| Active oxygen: | 13.4％ | 13.2％ | 13.4％ |
| Moisture content (175 ℃, 1 hour) | 1.47％ | 1.59％ | 1.37％ |
| Size distribution: | 0.5～1.0mm | 0.5～1.0mm | 0.5～1.0mm |
| Bulk density: kg/m3 | 1100 | 997 | 1056 |
| PH value: | 11.0 | 11.0 | 11.0 |
| Iron level: mg/kg | 12.2 | 14 | 13 |
| Dissolution rate: | 1 minute, 20% 3 minutes, 80% 5 minutes, 100% | 1 minute, 17% 3 minutes, 61% 5 minutes, 99% | 1 minute, 20% 3 minutes, 77% 5 minutes, 100% |
| Wet stability: | 76％ | 62％ | 70％ |
| Thermostability | 97％ | 94％ | 96％ |
Data from table can be seen, fast according to the coated SPC-D dissolution rate that the inventive method is produced, wet stability and thermostability have reached the advanced level of external like product all than higher, compare with domestic commercial like product, thermostability and wet stability all have bigger improvement.
Those of ordinary skill in the art will be appreciated that, above embodiment is used for illustrating the present invention, and be not as limitation of the invention, as long as in essential scope of the present invention, all will drop in the scope of claims of the present invention variation, the modification of the above embodiment.
Claims (2)
1. the preparation method of a particle type coating sodium percarbonate is characterized in that may further comprise the steps:
A. yellow soda ash, sodium-chlor, internal stabilizer are under agitation added formation yellow soda ash slip in the mother liquor that contains hydrogen peroxide 0.5%～1.0% (massfraction), yellow soda ash 6%～16% (massfraction), sodium-chlor 10%～20% (massfraction) by 100: 14～25: 0.5～5 mass ratio, temperature remains on 30～60 ℃;
Wherein, described internal stabilizer is tripoly phosphate sodium STPP, Trisodium Citrate, Starso, one or more in magnesium chloride or the sal epsom;
B. compound concentration is the hydrogen peroxide solution of 35% (massfraction), adds 1～4% (massfraction) stablizer; Described stablizer is one or more in ethylene diamine tetra methylene phosphonic acid, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, EDTA, sodium polyacrylate or the polyamide solution;
C. the throughput ratio of controlling yellow soda ash slip and hydrogen peroxide solution is 3: 1 (mass ratio), in the reactor of input tape agitator and cooling jacket;
D. controlling synthesis reaction temperature is 5～30 ℃, and the reaction times is 1～1.5 hour;
E. reaction is finished, and with the reaction product centrifugation, liquid phase is through filter press, the mother liquor reuse;
F. solid materials is removed surperficial moisture content through 80～120 ℃ of heat bakings, carries out the hydrojet dressing at fluidized-bed, gets particle type coating sodium percarbonate; Contain water glass (Na in the described hydrojet
2SiO
3), one or more outer stabilizers in sodium stearate, Natvosol, Sodium dodecylbenzene sulfonate, the sodium laurylsulfonate.
2. the preparation method of particle type coating sodium percarbonate as claimed in claim 1 is characterized in that in step c, adds the SPC-D nucleus in reactor.
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| CN104743518B (en) * | 2015-01-21 | 2017-02-22 | 江西省博浩源化工有限公司 | Application method of nucleation agent used for preparing sodium percarbonate |
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