CN110330023B - Preparation and drying method of magnesium trisilicate - Google Patents
Preparation and drying method of magnesium trisilicate Download PDFInfo
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- 239000000391 magnesium silicate Substances 0.000 title claims abstract description 73
- GXGAKHNRMVGRPK-UHFFFAOYSA-N dimagnesium;dioxido-bis[[oxido(oxo)silyl]oxy]silane Chemical compound [Mg+2].[Mg+2].[O-][Si](=O)O[Si]([O-])([O-])O[Si]([O-])=O GXGAKHNRMVGRPK-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 229940099273 magnesium trisilicate Drugs 0.000 title claims abstract description 70
- 229910000386 magnesium trisilicate Inorganic materials 0.000 title claims abstract description 70
- 235000019793 magnesium trisilicate Nutrition 0.000 title claims abstract description 70
- 238000001035 drying Methods 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 75
- 238000006243 chemical reaction Methods 0.000 claims abstract description 50
- 239000002245 particle Substances 0.000 claims abstract description 44
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 32
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 32
- 239000002253 acid Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 23
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 15
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 12
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 11
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 6
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 6
- 239000011734 sodium Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 105
- 239000000243 solution Substances 0.000 claims description 73
- 239000012295 chemical reaction liquid Substances 0.000 claims description 45
- 230000001502 supplementing effect Effects 0.000 claims description 44
- 239000002002 slurry Substances 0.000 claims description 40
- 239000000047 product Substances 0.000 claims description 32
- 238000001914 filtration Methods 0.000 claims description 29
- 239000007788 liquid Substances 0.000 claims description 27
- 239000012065 filter cake Substances 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 24
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 22
- 238000000926 separation method Methods 0.000 claims description 21
- 239000007921 spray Substances 0.000 claims description 17
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 239000008213 purified water Substances 0.000 claims description 14
- 239000004744 fabric Substances 0.000 claims description 13
- 238000003825 pressing Methods 0.000 claims description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 11
- 239000013522 chelant Substances 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 11
- 229910001385 heavy metal Inorganic materials 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 239000008187 granular material Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- 150000002500 ions Chemical class 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 230000009471 action Effects 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 7
- 238000005507 spraying Methods 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052785 arsenic Inorganic materials 0.000 claims description 6
- 229910052793 cadmium Inorganic materials 0.000 claims description 6
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000009826 distribution Methods 0.000 claims description 6
- 239000011777 magnesium Substances 0.000 claims description 6
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 6
- 229910021645 metal ion Inorganic materials 0.000 claims description 6
- 238000011085 pressure filtration Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 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 4
- RXDLGFMMQFNVLI-UHFFFAOYSA-N [Na].[Na].[Ca] Chemical compound [Na].[Na].[Ca] RXDLGFMMQFNVLI-UHFFFAOYSA-N 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims description 4
- 230000000903 blocking effect Effects 0.000 claims description 4
- 229940009662 edetate Drugs 0.000 claims description 4
- 229940113960 edetate calcium Drugs 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000005192 partition Methods 0.000 claims description 4
- 230000000717 retained effect Effects 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 229910052925 anhydrite Inorganic materials 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 3
- 238000013461 design Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 3
- NPUOZEMYDHAAMG-UHFFFAOYSA-N hexamagnesium;trisilicate Chemical compound [Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] NPUOZEMYDHAAMG-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 230000003472 neutralizing effect Effects 0.000 claims description 3
- 238000004537 pulping Methods 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 238000005265 energy consumption Methods 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000002955 isolation Methods 0.000 claims description 2
- 230000007246 mechanism Effects 0.000 claims description 2
- NVTRPRFAWJGJAJ-UHFFFAOYSA-L EDTA monocalcium salt Chemical compound [Ca+2].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O NVTRPRFAWJGJAJ-UHFFFAOYSA-L 0.000 claims 1
- 238000004891 communication Methods 0.000 claims 1
- 238000011049 filling Methods 0.000 claims 1
- 238000011010 flushing procedure Methods 0.000 claims 1
- 239000003595 mist Substances 0.000 claims 1
- 238000009987 spinning Methods 0.000 claims 1
- 239000007858 starting material Substances 0.000 abstract description 8
- 239000004576 sand Substances 0.000 abstract description 6
- 239000000825 pharmaceutical preparation Substances 0.000 abstract description 2
- SHWNNYZBHZIQQV-UHFFFAOYSA-J EDTA monocalcium diisodium salt Chemical compound [Na+].[Na+].[Ca+2].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O SHWNNYZBHZIQQV-UHFFFAOYSA-J 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 16
- 238000001514 detection method Methods 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 5
- 159000000003 magnesium salts Chemical class 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 235000014380 magnesium carbonate Nutrition 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical class [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- DNXIKVLOVZVMQF-UHFFFAOYSA-N (3beta,16beta,17alpha,18beta,20alpha)-17-hydroxy-11-methoxy-18-[(3,4,5-trimethoxybenzoyl)oxy]-yohimban-16-carboxylic acid, methyl ester Natural products C1C2CN3CCC(C4=CC=C(OC)C=C4N4)=C4C3CC2C(C(=O)OC)C(O)C1OC(=O)C1=CC(OC)=C(OC)C(OC)=C1 DNXIKVLOVZVMQF-UHFFFAOYSA-N 0.000 description 1
- 206010000087 Abdominal pain upper Diseases 0.000 description 1
- 241000185686 Apocynum venetum Species 0.000 description 1
- 241001106067 Atropa Species 0.000 description 1
- 206010020601 Hyperchlorhydria Diseases 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 206010067171 Regurgitation Diseases 0.000 description 1
- LCQMZZCPPSWADO-UHFFFAOYSA-N Reserpilin Natural products COC(=O)C1COCC2CN3CCc4c([nH]c5cc(OC)c(OC)cc45)C3CC12 LCQMZZCPPSWADO-UHFFFAOYSA-N 0.000 description 1
- QEVHRUUCFGRFIF-SFWBKIHZSA-N Reserpine Natural products O=C(OC)[C@@H]1[C@H](OC)[C@H](OC(=O)c2cc(OC)c(OC)c(OC)c2)C[C@H]2[C@@H]1C[C@H]1N(C2)CCc2c3c([nH]c12)cc(OC)cc3 QEVHRUUCFGRFIF-SFWBKIHZSA-N 0.000 description 1
- 239000004113 Sepiolite Substances 0.000 description 1
- 208000025865 Ulcer Diseases 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 229940069428 antacid Drugs 0.000 description 1
- 239000003159 antacid agent Substances 0.000 description 1
- 230000001458 anti-acid effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- SHWNNYZBHZIQQV-UHFFFAOYSA-L calcium;disodium;2-[2-[bis(carboxylatomethyl)azaniumyl]ethyl-(carboxylatomethyl)azaniumyl]acetate Chemical compound [Na+].[Na+].[Ca+2].[O-]C(=O)C[NH+](CC([O-])=O)CC[NH+](CC([O-])=O)CC([O-])=O SHWNNYZBHZIQQV-UHFFFAOYSA-L 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- -1 compound aluminum hydroxide Chemical class 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 201000006549 dyspepsia Diseases 0.000 description 1
- 229910052839 forsterite Inorganic materials 0.000 description 1
- 210000004211 gastric acid Anatomy 0.000 description 1
- 208000024798 heartburn Diseases 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007415 particle size distribution analysis Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- BJOIZNZVOZKDIG-MDEJGZGSSA-N reserpine Chemical compound O([C@H]1[C@@H]([C@H]([C@H]2C[C@@H]3C4=C([C]5C=CC(OC)=CC5=N4)CCN3C[C@H]2C1)C(=O)OC)OC)C(=O)C1=CC(OC)=C(OC)C(OC)=C1 BJOIZNZVOZKDIG-MDEJGZGSSA-N 0.000 description 1
- 229960003147 reserpine Drugs 0.000 description 1
- MDMGHDFNKNZPAU-UHFFFAOYSA-N roserpine Natural products C1C2CN3CCC(C4=CC=C(OC)C=C4N4)=C4C3CC2C(OC(C)=O)C(OC)C1OC(=O)C1=CC(OC)=C(OC)C(OC)=C1 MDMGHDFNKNZPAU-UHFFFAOYSA-N 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- 238000005029 sieve analysis Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical group [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 231100000397 ulcer Toxicity 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D25/00—Filters formed by clamping together several filtering elements or parts of such elements
- B01D25/12—Filter presses, i.e. of the plate or plate and frame type
- B01D25/21—Plate and frame presses
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/22—Magnesium silicates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention belongs to the technical field of pharmaceutical preparation, and provides a method for preparing and drying magnesium trisilicate, which comprises the following raw materials: boiler scale1000 portions of 1500 portions of sodium silicate, 50 portions to 100 portions of acid solution and sodium silicate (Na)2O·nSiO2)60-120 parts of sodium hydroxide (NaOH)90-180 parts of calcium disodium edetate (CaNa)2EDTA)30-60 parts; the main component in the boiler scale contains Mg2+、Ca2+、Mg(OH)2、CaCO3And a small amount of MgCO3The method for preparing and drying magnesium trisilicate of the present invention begins with collecting boiler scale raw material through S1 until the product of magnesium trisilicate is dried through S10; provides a preparation method and a drying method of magnesium trisilicate, which have the advantages of low cost of starting materials, mild reaction conditions, more uniform product shape and particles, high acid making capacity and no sand.
Description
Technical Field
The invention belongs to the technical field of pharmaceutical preparation, and particularly relates to a method for preparing and drying magnesium trisilicate.
Background
Magnesium trisilicate, also known as "orthomagnesium silicate", of the formula Mg2Si3O8.nH2O, is a white fine powder which has no gritty feel and is decomposed in concentrated alkali to form Mg (OH)2, which is decomposed in hot hydrochloric acid to form silicic acid and magnesium chloride, which can be decomposed by hydrofluoric acid. The forsterite mineral exists in nature. The magnesium trisilicate has good adsorption performance and molecular sieve function, can provide specific molecular field acting force, is used for preparing antacid in medicine, can neutralize gastric acid and protect ulcer surface, has slow and lasting action, and is used for relieving stomachache, heartburn and acid regurgitation caused by hyperchlorhydria. It is used as anticaking agent, filter aid and coating agent in food industry, and is mainly used for compound aluminum hydroxide tablet, vitamin u belladonna aluminum magnesium tablet, compound reserpine, compound apocynum venetum and other compound preparations. In addition, it can be used as deodorizing agent, decoloring agent, etc., and in ceramics and rubber industry. The crystal structure of the magnesium trisilicate is similar to the crystal structure of sepiolite 2:1 type chain and layered transition type, and currently, magnesium trisilicate is prepared by precipitation method by using magnesium nitrate, magnesium oxide and sodium silicate as raw materials in the main industry. Some starting materials in the preparation methods are not easy to obtain, some starting materials have high cost, some process operations are complex, some properties of the obtained product are large in particle size, and other manufacturers adopt white fine powder which is obtained after spray drying, has grittiness and does not meet the requirements of Chinese pharmacopoeia standards and has no grittiness feeling.
Therefore, in order to solve the above problems, it is necessary to design a method for preparing magnesium trisilicate and a drying method thereof, which have low cost of starting materials, more uniform product shape particles, high acid making capacity and no sand, and meet the requirements of Chinese pharmacopoeia standards.
Disclosure of Invention
The invention overcomes the defects of the prior art, and aims to provide a preparation method which has the advantages of low cost of starting materials, mild reaction conditions, more uniform product-shaped particles, high acidity production and no sand, and particularly provides a suitable starting material, a suitable material molar ratio, a suitable drying mode and a scheme which can ensure that the prepared product-shaped particles are uniform, so that the magnesium trisilicate properties meet the standard of Chinese pharmacopoeia, the ratio of silicon dioxide to magnesium oxide is moderate, and the acidity production is high. The main chemical reaction formula of the application is as follows:
2Mg2++Na2O·nSiO2→2MgO·3SiO2·nH2O+2Na+
the present invention solves the above problems by the following techniques:
first, relevant raw materials are collected, the raw materials including: 1000-1500 parts of boiler scale, 50-100 parts of acid solution and sodium silicate (Na)2O·nSiO2)60-120 parts of sodium hydroxide (NaOH)90-180 parts of calcium disodium edetate (CaNa)2EDTA)30-60 parts; the main component in the boiler scale contains Mg2+、Ca2+、Mg(OH)2、CaCO3And a small amount of MgCO3Simultaneously contains trace heavy metal ion cadmium Cd2+Aluminum Al3+As, As3+Hg, Hg2+(ii) a Compared with the traditional preparation of magnesium salts in magnesium trisilicate, the method for extracting magnesium sulfate from boiler scale has the advantages that raw materials are convenient to obtain, on one hand, the cost of the raw materials can be effectively reduced, and simultaneously, substances in the scale are effectively recycled, so that the method is a good attempt for waste utilization and has important significance, and the method is a good breakthrough and innovation for preparing magnesium trisilicate; the selection of disodium calcium edetate can well neutralize heavy metal ions in the water scale, so that the defect of preparing magnesium trisilicate from boiler water scale is overcome; the preparation and drying method comprises the following steps:
s1, storing a certain amount of boiler scale through a large-scale recovery mode; taking 1000-1500 parts of boiler scalePretreating the selected boiler scale, including screening and drying, crushing into granules of 3-5cm, and putting into an ultrafine crushing device until the granules are ultrafine-crushed into 100-mesh granules to form boiler scale powder, wherein the powdery form is convenient for better chemical reaction; because the highest component in the boiler scale is CaCO3And the second component is Mg (OH)2Therefore, taking as much boiler scale as possible helps to extract more MgSO4Preparing and using magnesium salt;
s2, putting the boiler scale powder in the S1 into a water storage tank which is prepared in advance, adding a certain amount of aqueous solution, and then stirring to form boiler scale powder slurry;
s3, adding a certain amount of disodium calcium edetate (CaNa) into the slurry formed in the step S22EDTA), heavy metal ion cadmium Cd of disodium edetate calcium boiler scale powder slurry2+Aluminum Al3+As, As3+Hg, Hg2+Neutralizing to form a stable and soluble metal chelate, and including each metal ion into the chelate to form a stable compound with larger molecular weight, so that the metal ions are prevented from acting in subsequent chemical reactions, and the influence of heavy metal substances on human bodies is avoided; the finally formed metal chelate is discharged through the human body, and cannot be retained in the human body to cause potential safety hazards;
s4, adding a certain amount of acid solution into the slurry reacted in the step S3, wherein the acid solution is Mg (OH)2、CaCO3And a small amount of MgCO3All the components are subjected to acidolysis to form a product solution after acidolysis; the acid solution is concentrated sulfuric acid H2SO4At this time, the main substance reaction formula of acidolysis is:
Mg(OH)2+H2SO4＝MgSO4+2H2O
CaCO3+H2SO4＝CaSO4+H2O
MgCO3+H2SO4＝MgSO4+H2O+CO2↑
s5, passing through S4 filtering the product solution after the acidolysis reaction so as to remove CaSO in the product solution4Filtered off to form MgSO containing only the stable metal chelate4A solution; to this end, a transition from boiler scale to MgSO is achieved4Magnesium salt is well refined, so that the boiler scale can be well recycled;
s6, MgSO (MgSO) as described in S54Adding a quantity of water to the solution to form MgSO in accordance with the preparation concentration of the magnesium trisilicate4A solution;
s7, respectively preparing a certain amount of sodium silicate solution and a certain amount of sodium hydroxide solution, standing the sodium silicate solution, fully settling the sodium silicate solution, and mixing the sodium silicate solution with the sodium hydroxide solution;
s8, adding a certain amount of MgSO 6 in the step S6 into a reaction kettle prepared in advance4Adding the mixed solution of sodium silicate and sodium hydroxide obtained in the step S7 into the solution, and stirring for reaction after the addition is finished;
s9, pumping the reaction liquid obtained in the step S8 into a plate frame of a plate-and-frame filter press prepared in advance, washing with purified water, after the first washing is finished, discharging a pressing plate for pulping, pumping the pulp into the plate frame of a clean area, continuing to perform secondary washing, and discharging the pressing plate after the washing is finished;
s10, sampling and controlling, drying after the free alkali is qualified, and finally obtaining the magnesium trisilicate which has low cost, high acid making capacity and no sand and meets the standard requirements of Chinese pharmacopoeia.
Further, the concentration of the sodium silicate solution is 15% -25%, and MgSO is used in the step S64The concentration of the solution is 15-20%, and the concentration of the sodium hydroxide is 15-20%.
Further, the preparation method comprises the following steps: MgSO (MgSO)4: sodium silicate: sodium hydroxide ═ 1: (1.5-2.0): (2.5-3.0) and the reaction temperature is 10-60 ℃.
Further, the concentration of the sodium silicate solution is preferably 25% -30%, MgSO4The concentration of the solution is preferably 20-30%, and the concentration of sodium hydroxide is 20-30%.
Further, the feeding molar ratio is more preferably MgSO4Solution:sodium silicate: sodium hydroxide ═ 1: 1.8: 2.7, the reaction temperature is preferably 30-40 ℃; repeated experiments show that the magnesium trisilicate has the highest acid making capacity and the best quality under the molar ratio.
Further, the control range of the pH value of the controlled free alkali is 8-12, and the more preferable control range is 9-10.
Further, the drying manner may be vacuum drying, forced air drying, double cone drying and flash evaporation drying.
Further, the drying temperature of the vacuum drying, the forced air drying and the double cone drying is 30-80 ℃, the air inlet temperature of the flash drying is 200-260 ℃, the air outlet temperature is 60-110 ℃, the feeding frequency is 5-25Hz, the preferable air inlet temperature is 240-250 ℃, the air outlet temperature is 95-105 ℃ and the feeding frequency is 15-25 Hz.
Further, the plate-and-frame filter press in the step S9 of the present invention includes a frame 1, a slide rail 11, a control box 12, an oil cylinder 13, and an oil supply unit 14; one end of the rack 1 is fixedly connected with an oil supply unit 14, and the oil supply unit 14 is connected with a power supply through a control box 12 on the rack 1; one side of the frame 1, which is far away from the oil supply unit 14, is fixedly connected with a fixed plate 15 through a pair of slide rails 11; one side of the slide rail 11 close to the fixed plate 15 is connected with a shunting block 2 in a sliding manner, and the slide rail 11 at one side of the shunting block 2 far away from the fixed plate 15 is connected with a group of filter plates 3 in a sliding manner; a pressing plate 16 is connected to the slide rail 11 on one side of the filter plate 3 close to the oil supply unit 14 in a sliding manner, and the pressing plate 16 is driven by an oil cylinder 13 fixedly connected to the frame 1; the oil cylinder 13 is communicated with an oil supply unit 14 through a pipeline; a feed pipe 17 is fixedly connected to one side of the fixing plate 15, which is far away from the shunting block 2, and high-pressure reaction liquid flows into the shunting block 2 through the feed pipe 17; a cylindrical separation cavity 21 is arranged in the shunting block 2, and a funnel-shaped separation barrel 22 is rotatably connected in the separation cavity 21; a rotating shaft at the bottom of the separating cylinder 22 is fixedly connected with an output shaft of a motor 23 fixedly connected to the bottom of the shunting block 2; the feeding pipe 17 is communicated with the separation cavity 21 through a feeding hole 24 on the shunting block 2, and the height of the feeding hole 24 is higher than the upper edge of the separation cylinder 22; the separation cylinder 22 and the separation cavity 21 are divided into four chambers 26 by a group of partition plates 25 fixedly connected with the inner wall of the separation cavity 21, and each chamber 26 is communicated with the filter plate 3 by a respective communicating pipe 27; the isolation plate 25 is connected with the separation cylinder 22 in a sliding and sealing manner; a group of filtering holes 28 are uniformly formed in the circumference of the separating cylinder 22 between the adjacent partition plates, and the diameters of the four groups of filtering holes 28 are sequentially increased from top to bottom; a groove 31 is formed on one side of the adjacent filter plates 3, which is in contact with the filter plates, and filter cloth 32 is arranged in the groove 31; a group of water filtering grooves 33 are uniformly formed in the bottom of the groove 31, and the water filtering grooves 33 are communicated with a water collecting pipe 35 below the filter plate 3 through a collecting pipe 34; the collecting pipe 34 is connected with an air source through an air supply pipe 36 on the filter plate 3 by a valve; a first slurry supplementing hole 37, a second slurry supplementing hole 38, a third slurry supplementing hole 39 and a fourth slurry supplementing hole 310 are sequentially formed in the upper part of the filter plate 3; the filter plate 3 is divided into a group A, a group B, a group C and a group D in sequence from one side close to the flow distribution block 2; the first pulp supplementing hole 37 is communicated with the groove 31 of the group A filter plate 3, the second pulp supplementing hole 38 is communicated with the groove 31 of the group B filter plate 3, the third pulp supplementing hole 39 is communicated with the groove 31 of the group C filter plate 3, and the fourth pulp supplementing hole 310 is communicated with the groove 31 of the group D filter plate 3; butterfly valves 311 for controlling the corresponding first slurry supplementing hole 37, second slurry supplementing hole 38, third slurry supplementing hole 39 and fourth slurry supplementing hole 310 are arranged on the filter plates 3 adjacent to the group A and the group B, the group B and the group C and the group D; the first slurry supplementing hole 37, the second slurry supplementing hole 38, the third slurry supplementing hole 39 and the fourth slurry supplementing hole 310 are respectively communicated with the communicating pipe 27 at the corresponding position on the flow dividing block 2; the filter plate 3 is also provided with a group of water supply holes 312, and the water supply holes 312 are communicated with a pressure water source through a water pipe and a control valve; the water supply hole 312 communicates with the groove 31; the water collecting pipe 35 is communicated with an air source through an air pipe and an electromagnetic valve;
when the material pressing and filtering are needed, the oil supply unit 14 is started through the control box 12, the oil cylinder 13 is driven to press the filter plates 3 and the diverter 2, then the reaction material liquid in the step S8 is sent into the separating cylinder 22 in the separating cavity 21 through the feed pipe 17 and the feed hole 24 under high pressure, simultaneously, the motor 23 is started to drive the separating cylinder 22 to rotate, under the action of centrifugal force, the rotating separating cylinder 22 separates particles with different sizes in the reaction material liquid due to different centrifugal force action on the particles with different sizes, wherein the magnesium trisilicate particles in the reaction material liquid are increased in diameter from top to bottom in the separating cylinder 22, the particles with larger diameter in the reaction material liquid flow into the cavity 26 at the corresponding position from the filtering hole 28 at the lower part of the separating cylinder 22, the particles with smaller diameter in the reaction material liquid flow into the cavity 26 at the corresponding position from the filtering hole 28 at the upper part of the separating cylinder 22 under the action of centrifugal force, separated reaction liquid with different particle sizes respectively flows into the grooves 31 in the corresponding groups of filter plates 3 through the first pulp supplementing hole 37, the second pulp supplementing hole 38, the third pulp supplementing hole 39 and the fourth pulp supplementing hole 310, the reaction liquid flows into the cavities formed by the grooves 31 and the filter cloth 32 in the adjacent filter plates 3, at the moment, the reaction liquid in the feeding pipe 17 is continuously pressurized, so that water in the reaction liquid between the adjacent filter cloth 32 is extruded to form filter cakes, the extruded water is collected by the collecting pipe 34 and flows into the water collecting pipe 35 to be recovered, then the oil cylinder 13 is controlled by the control box 12 to retract, purified water is introduced into the water supply hole 312 after the adjacent filter plates 3 are separated, the filter cakes formed in the grooves 31 are washed, then the oil cylinder 13 is controlled by the control box 12 to tightly press the filter plates 3, then the pressure reaction liquid is continuously pumped into the grooves 31 in the filter plates 3 to continuously extrude the water, then the oil cylinder 13 is withdrawn, and the purified water is introduced through the water supply hole 312 to wash, finally, a valve is opened to supply air to the air supply pipe 36, high-pressure air is filled between the filter cloth 32 and the groove 31 through the collecting pipe 34, so that the filter cake is separated from the groove 31 after the filter cloth 32 is expanded, and the filter cake falls off.
Because the diameters of the particles in the reaction feed liquid introduced into the group A, group B, group C and group D filter plates 3 are different, the diameters of the magnesium trisilicate particles in the filter cakes generated by the group A, group B, group C and group D filter plates 3 are different, but the diameters of the magnesium trisilicate particles in the filter cakes in the same group of filter plates 3 are relatively uniform, and then, external personnel store the magnesium trisilicate generated by different groups in batches; the design of this mechanism of this application for the categorised comparatively even of magnesium trisilicate diameter after the filter-pressing of plate and frame filter press in this application, the uneven condition of a batch diameter can not appear.
Meanwhile, the filter cake formed by particles with smaller diameters does not need to be ground, the subsequent grinding work is reduced, the production cost is saved, meanwhile, the shunting block 2 is in close contact with the filter plate 3, the transportation distance of the reaction liquid after shunting is reduced, and the resistance of the reaction liquid on the pipeline wall in the flowing process is reduced, so that the pressure loss is reduced, the energy is saved, the purchase of connecting pipes can be reduced, the equipment cost is reduced, meanwhile, the connecting link of the force shunting block 2 and the filter plate 3 is reduced, and the possibility of leakage is reduced.
A cam 4 is fixedly connected to a rotating shaft at the bottom of the separating cylinder 22, and a cylinder 41 is arranged at the bottom of the separating cavity 21 and corresponds to the cam 4; a first piston rod 42 in the cylinder 41 is in contact connection with the cam 4, and a spring is arranged in a rodless cavity of the cylinder 41; the butterfly valve 311 is a pneumatic valve, and the butterfly valve 311 is communicated with the rodless cavity of the cylinder 41 through a pipeline.
When the reaction liquid particles are even, when the split flow is not needed, high-pressure reaction liquid flows into the separating cylinder 22 in the separating cavity 21 through the feeding pipe 17 and the feeding hole 24, the motor 23 is not started at the moment, the separating cylinder 22 does not rotate, the reaction liquid flows to the filter plates 3 from all the cavities 26 through the communicating pipe 27 uniformly, the moisture filtration is carried out, the cam 4 does not rotate at the moment, the air cylinder 41 does not generate compressed gas, all the butterfly valves 311 are opened under the pressure effect of the reaction liquid after losing the air supply, the reaction liquid flows into all the filter plates 3, the moisture filtering operation is carried out, when different particle diameters in the reaction liquid need to be separated, the motor 23 is started to drive the cam 4 to rotate, the air cylinder 41 generates the compressed gas to drive the butterfly valves 311 to be closed, and the reaction liquid with different particle diameters can be.
One side of the filter plate 3 close to the groove 31 is uniformly provided with a group of horizontally arranged piston cylinders 5, and a second piston rod 51 is connected in the piston cylinders 5 in a sliding manner; one end of the second piston rod 51, which is positioned outside the piston cylinder 5, faces the adjacent filter plate 3; a return spring 52 is arranged in a rodless cavity of the piston cylinder 5; a rod cavity of the piston cylinder 5 is communicated with the groove 31 through a pressurizing hole 53, and the pressurizing hole 53 penetrates through the filter cloth 32; a fastening cavity 54 is formed in the position, corresponding to the second piston rod 51, of the adjacent filter plate 3, and a clamping block 55 is rotatably connected in the fastening cavity 54; a clamping groove 56 is formed in the position, corresponding to the clamping block 55, of the second piston rod 51, and when the filter plate 3 is pressed tightly, the clamping block 55 rotates to clamp the clamping groove 56; the rotating shaft of the fixture block 55 is sleeved with a torsion spring for resetting the fixture block 55; and a handle 57 is fixedly connected to one end of the rotating shaft of the clamping block 55, which extends out of the filter plate 3.
After the adjacent filter plates 3 are tightly extruded, the other clamping grooves 56 of the second piston rod 51 are clamped by the clamping blocks 55, high-pressure reaction liquid is filled in the grooves 31, the reaction liquid enters the rodless cavity of the piston cylinder 5 through the pressurizing holes 53 at the moment, the second piston rod 51 is pulled, the adjacent filter plates 3 are extruded more tightly, the probability of leakage of the reaction liquid from gaps between the adjacent filter plates 3 is reduced, the reaction force between the squeezing pressure of the filtering press and the sealing pressure of the grooves 31 is reduced, the kinetic energy consumption is reduced, and the energy is saved.
The rod cavity of the piston cylinder 5 is communicated with the water supply hole 312 through a valve of the water spray hole 58, and the water spray hole 58 is used for spraying clean water to clean the inner wall of the piston cylinder 5; purified water in the water supply holes 312 is sprayed into the piston cylinder 5 through the water spray holes 58, reaction liquid participating in the piston cylinder 5 is cleaned, the reaction liquid is prevented from blocking the second piston rod 51 to move, the condition that the piston cylinder 5 is inconvenient to use for the second time is avoided, and meanwhile, the condition that magnesium trisilicate cannot fall off in the follow-up cleaning process due to the fact that the magnesium trisilicate reaction liquid is retained in the piston cylinder is avoided, so that the magnesium trisilicate is wasted.
The water spray holes 58 are communicated with air spray holes 59, and the air spray holes 59 are communicated with the collecting main 34 through pipelines and valves; the air injection holes 59 inject air into the water injection holes 58, water is atomized and then is injected out, and the cleaning effect of the piston cylinder 5 is improved; jet to the hole for water spraying 58 through the fumarole 59 for the water in the hole for water spraying 58 spouts after the atomizing, and the water economy is used water consumption, increases out water velocity simultaneously, and the participation reaction feed liquid in the further clearance piston cylinder 5 prevents that the reaction feed liquid from hindering No. two piston rod 51 motion.
The water spray holes 58 are arranged along the tangential direction of the inner wall of the piston cylinder 5, and water flow sprayed out of the water spray holes 58 is sprayed out along the inner wall of the piston cylinder 5 to form wheel swirling water flow, so that the cleaning dead angle in the piston cylinder 5 is reduced; through the hole for water spraying 58 with the tangential direction of the inner wall of the piston cylinder 5 arranges for spun rivers and water smoke form spiral rivers at the inner wall of the piston cylinder 5, increase the cleaning area and the cleaning efficiency, reduce the clearance dead angle in the piston cylinder 5, further prevent that the reaction feed liquid from hindering the motion of No. two piston rods 51.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a process for preparing and drying the magnesium trisilicate, which has the advantages of low cost of starting materials, mild reaction conditions, more uniform product-shaped particles, high acid making capacity of the product and good fluidity and is free of sand;
2. the invention adopts boiler scale as the initial raw material to prepare MgSO in a breakthrough manner4The magnesium salt changes the traditional thinking of preparing the magnesium salt by using magnesite, magnesia and other materials, has convenient raw material acquisition, can effectively reduce the cost of the raw material on one hand, and simultaneously effectively recycles substances in the scale, is an attempt for good utilization of waste, and has important significance;
3. the invention adopts boiler scale as the initial raw material in a breakthrough manner, and simultaneously considers heavy metal ion cadmium Cd possibly carried in the scale2+Aluminum Al3+As, As3+Hg, Hg2+Will bring potential safety hazard to human body, therefore, disodium edetate calcium (CaNa) is added in the preparation process2EDTA), the potential safety hazard brought to people by the heavy metal ions is effectively avoided, and the practicability and the rationality of the invention are improved;
4. in order to solve the problem of uneven product shape particles, the invention adopts a unique plate-and-frame filter press structure, and can divide magnesium trisilicate with different diameters into four batches in the process of magnesium trisilicate filter pressing, and each batch is placed independently, thereby effectively avoiding the situation that the same magnesium trisilicate product has uneven particle size; thereby effectively improving the product quality of the magnesium trisilicate.
Drawings
The invention will be further explained with reference to the drawings.
FIG. 1 is a graph showing the cumulative particle size characteristics of the present invention measured by particle size distribution analysis;
FIG. 2 is a schematic view of the overall structure of the plate-and-frame filter press of the present invention;
figure 3 is a side view of the plate and frame filter press of the present invention;
figure 4 is a cross-sectional view of a diverter block of a plate and frame filter press of the present invention;
figure 5 is a front view of a filter plate of the plate and frame filter press of the present invention;
FIG. 6 is a cross-sectional view of a filter plate of a plate and frame filter press in contact with a spacer plate according to the present invention;
FIG. 7 is an enlarged view at E of FIG. 6;
fig. 8 is an enlarged view at F in fig. 6.
In the figure: the device comprises a frame 1, a slide rail 11, a control box 12, an oil cylinder 13, an oil supply unit 14, a fixing plate 15, a flow dividing block 2, a filter plate 3, a pressing plate 16, a feed pipe 17, a separation cavity 21, a separation cylinder 22, a motor 23, a feed hole 24, a separation plate 25, a cavity 26, a communicating pipe 27, a filter hole 28, a groove 31, filter cloth 32, a water filtering groove 33 and a collecting pipe 34, the device comprises a water collecting pipe 35, an air supply pipe 36, a first slurry supplementing hole 37, a second slurry supplementing hole 38, a third slurry supplementing hole 39, a fourth slurry supplementing hole 310, a butterfly valve 311, a water supply hole 312, a cam 4, an air cylinder 41, a first piston rod 42, a piston cylinder 5, a second piston rod 51, a return spring 52, a pressurizing hole 53, a fastening cavity 54, a fixture block 55, a clamp groove 56, a handle 57, a water spraying hole 58 and an air spraying hole 59.
Detailed Description
Referring to fig. 1 to 8, a method for preparing and drying magnesium trisilicate according to an embodiment of the present invention is described as follows:
the preparation and drying method of magnesium trisilicate comprises the following steps:
s1, storing a certain amount of boiler scale through a large-scale recovery mode; taking 1000-1500 parts of the boiler scale, carrying out pretreatment on the selected boiler scale, including screening and drying treatment, crushing the boiler scale into granules of 3-5cm, and putting the granules into ultrafine crushing equipment until the granules are ultrafine crushed into granules with the size of 100 meshes to form boiler scale powder, wherein the powdery form is convenient for better chemical reaction; because the highest component in the boiler scale is CaCO3And the second component is Mg (OH)2Therefore, taking as much boiler scale as possible helps to extract more MgSO4Preparing and using magnesium salt;
s2, putting the boiler scale powder in the S1 into a water storage tank which is prepared in advance, adding a certain amount of aqueous solution, and then stirring to form boiler scale powder slurry;
s3, adding a certain amount of disodium calcium edetate (CaNa) into the slurry formed in the step S22EDTA), heavy metal ion cadmium Cd of disodium edetate calcium boiler scale powder slurry2+Aluminum Al3+As, As3+Hg, Hg2+Neutralizing to form a stable and soluble metal chelate, and including each metal ion into the chelate to form a stable compound with larger molecular weight, so that the metal ions are prevented from acting in subsequent chemical reactions, and the influence of heavy metal substances on human bodies is avoided; the finally formed metal chelate is discharged through the human body, and cannot be retained in the human body to cause potential safety hazards;
s4, adding a certain amount of acid solution into the slurry reacted in the step S3, wherein the acid solution is Mg (OH)2、CaCO3And a small amount of MgCO3All the components are subjected to acidolysis to form a product solution after acidolysis; the acid solution is concentrated sulfuric acid H2SO4At this time, the main substance reaction formula of acidolysis is:
Mg(OH)2+H2SO4＝MgSO4+2H2O
CaCO3+H2SO4＝CaSO4+H2O
MgCO3+H2SO4＝MgSO4+H2O+CO2↑
s5, filtering the product solution subjected to the acidolysis reaction of S4 to obtain CaSO in the product solution4Filtered off to form MgSO containing only the stable metal chelate4A solution; to this end, a transition from boiler scale to MgSO is achieved4Magnesium salt is well refined, so that the boiler scale can be well recycled;
s6, MgSO (MgSO) as described in S54Adding a quantity of water to the solution to form MgSO in accordance with the preparation concentration of the magnesium trisilicate4A solution;
s7, respectively preparing a certain amount of sodium silicate solution and a certain amount of sodium hydroxide solution, standing the sodium silicate solution, fully settling the sodium silicate solution, and mixing the sodium silicate solution with the sodium hydroxide solution;
s8, adding a certain amount of MgSO 6 in the step S6 into a reaction kettle prepared in advance4Adding the mixed solution of sodium silicate and sodium hydroxide obtained in the step S7 into the solution, and stirring for reaction after the addition is finished;
s9, pumping the reaction liquid obtained in the step S8 into a plate frame of a plate-and-frame filter press prepared in advance, washing with purified water, after the first washing is finished, discharging a pressing plate for pulping, pumping the pulp into the plate frame of a clean area, continuing to perform secondary washing, and discharging the pressing plate after the washing is finished; the specific structure and effect of the plate filter press are described in the above related contents of the present application.
S10, sampling and controlling, drying after the free alkali is qualified, and finally obtaining the magnesium trisilicate which has low cost, high acid making capacity and no sand and meets the standard requirements of Chinese pharmacopoeia.
In order to verify the effect of the magnesium trisilicate product, the following test operations of a control group 1 to an experimental group 5 were carried out by the personnel related to the application:
TABLE 1-number of Components in the preparation of magnesium trisilicate in the manner described herein
The experimental conditions of the above examples are as follows:
Weighing 100g of MgSO 20% strength MgSO prepared by traditional magnesite material4Adding the solution into a 500ml three-necked bottle, adding 180g of sodium silicate solution with the concentration of 25% and 270g of sodium hydroxide solution with the concentration of 20% into a reaction bottle, stirring for 5 hours at 50 ℃, filtering to obtain magnesium trisilicate pressure liquid, performing pressure filtration on the prepared magnesium trisilicate pressure liquid by using a conventional plate-and-frame filter press to obtain a filter cake, leaching the filter cake by using purified water of the plate-and-frame filter press for four times, controlling the pH (9-10) of free alkali to be qualified, and drying conventionally to obtain a magnesium trisilicate product.
100g of 20% MgSO prepared from boiler scale material of the present application was weighed out4Adding the solution into a 500ml three-necked bottle, adding 180g of sodium silicate solution with the concentration of 25% and 270g of sodium hydroxide solution with the concentration of 20% into a reaction bottle, stirring for 5 hours at 50 ℃, filtering to obtain magnesium trisilicate pressure liquid, performing pressure filtration on the prepared magnesium trisilicate pressure liquid by using a conventional plate-and-frame filter press to obtain a filter cake, leaching the filter cake by using purified water of the plate-and-frame filter press for four times, controlling the pH (9-10) of free alkali to be qualified, and drying conventionally to obtain a magnesium trisilicate product.
100g of 20% MgSO prepared from boiler scale material of the present application was weighed out4Adding the solution into a 500ml three-necked bottle, adding 150g of sodium silicate solution with the concentration of 25% and 250g of sodium hydroxide solution with the concentration of 20% into a reaction bottle, stirring for 5 hours at 50 ℃, filtering to obtain magnesium trisilicate pressure liquid, performing pressure filtration on the prepared magnesium trisilicate pressure liquid by using the plate-and-frame filter press to obtain a filter cake, leaching the filter cake by using purified water of the plate-and-frame filter press for four times, controlling the pH (9-10) of free alkali to be qualified, and drying by using the double-cone mode to obtain a magnesium trisilicate product.
100g of 20% MgSO prepared from boiler scale material of the present application was weighed out4Adding the solution into a 500ml three-necked bottle, adding 180g of sodium silicate solution with the concentration of 25% and 270g of sodium hydroxide solution with the concentration of 20% into a reaction bottle, stirring for 5 hours at 50 ℃, filtering to obtain magnesium trisilicate pressure liquid, performing pressure filtration on the prepared magnesium trisilicate pressure liquid by using the plate-and-frame filter press to obtain a filter cake, leaching the filter cake by using purified water of the plate-and-frame filter press for four times, controlling the pH (9-10) of free alkali to be qualified, and drying by using the double-cone mode to obtain a magnesium trisilicate product.
100g of 20% MgSO prepared from boiler scale material of the present application was weighed out4Adding the solution into 500ml three-neck flask, adding 200g sodium silicate solution with 25% concentration and 300g sodium hydroxide solution with 20% concentration into reaction flask, stirring at 50 deg.C for 5 hr, filtering to obtain magnesium trisilicate pressure liquid, and mixing with the pressure liquidThe prepared magnesium trisilicate pressure liquid is subjected to pressure filtration by using the plate-and-frame filter press to obtain a filter cake, the filter cake is leached by using purified water of the plate-and-frame filter press for four times, the pH (9-10) of free alkali is controlled to be qualified, and then the magnesium trisilicate product is obtained after drying by using the double-cone mode.
Detection format: the magnesium trisilicate products obtained in the control group 1 to the experimental group 5 are subjected to result detection, and the main detection items are acid making force detection, ignition weightlessness detection and product particle size detection.
Test equipment: the acid making power is detected by adopting a third method device of XC dissolution measurement method in the appendix of 2010 edition (second part) of Chinese pharmacopoeia, and the burning weight loss is detected by adopting a drying weight loss measurement method in 2015 edition (fourth part) of Chinese pharmacopoeia; since the above detection method is prior art, it will not be elaborated herein too much; it should be noted that, in the product particle detection, 50g of magnesium trisilicate product is selected from the control group 1 to the experimental group 5, the particle size distribution is detected by a conventional sieve analysis method, and a cumulative particle size characteristic curve is drawn.
And (3) test results: the acidity, ignition loss and particle size distribution of the magnesium trisilicate products in the different experiments are shown in Table 2.
TABLE 2-SALICIUM SALICIDE PRODUCTS ACID-MAKING POWER, DEW OF GLOW AND STRENGTH DISTRIBUTION CONDITIONS TABLE
Note: the specific condition of the product particle size distribution refers to the attached figure 1 of the specification, the actually measured data in the test has partial errors, the error range is controllable, and the final experimental analysis is not influenced.
Analysis was performed from the above 3 items of test data:
(1) the analysis of control 1 and control 2 gave MgSO 4, which was prepared from the boiler scale material of the present application4MgSO prepared relative to traditional magnesite material4，MgSO4There is no actual difference in quality of (A);
(2) the comparison group 1 and the experiment group 4 are used for analysis, so that the quality of the magnesium trisilicate product prepared by the method is better than that of the magnesium trisilicate prepared by the traditional method, and the acid making capacity is higher;
(3) the analysis of experimental group 3, experimental group 4 and experimental group 5 shows that the molar ratio of the materials fed in the process of preparing magnesium trisilicate is more preferably MgSO4Solution: sodium silicate: sodium hydroxide ═ 1: 1.8: 2.7, the prepared magnesium trisilicate has the best quality and the highest acid making capacity;
(4) by comparing the comparison groups 1-2 with the experiment groups 3-5, the magnesium trisilicate product obtained by adopting the plate-and-frame filter press to filter press has more uniform particle size.
In conclusion, the invention provides a sand-free magnesium trisilicate preparation and drying process which has the advantages of low cost of starting materials, mild reaction conditions, uniform product shape and particles and high acid-making capacity of the product.
In the description of the present invention, it is to be understood that the indicated orientations or positional relationships are based on the orientations or positional relationships shown in the drawings and are only for convenience in describing the present invention and simplifying the description, but are not intended to indicate or imply that the indicated devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be taken as limiting the scope of the present invention.
While the invention has been described with reference to specific embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (3)
1. A method for preparing and drying magnesium trisilicate is characterized in that: the raw materials comprise: 1000-1500 parts of boiler scale, 50-100 parts of acid solution and sodium silicate (Na)2O·nSiO2)60-120 parts of sodium hydroxide (NaOH)90-180 parts of calcium disodium edetate (CaNa)2EDTA)30-60 parts; the main chemical component in the boiler scale contains Mg2＋、Ca2＋、Mg(OH)2、CaCO3And a small amount of MgCO3Simultaneously contains trace heavy metal ion cadmium Cd2＋Aluminum Al3＋As, As3＋Hg, Hg2＋(ii) a The preparation and drying method comprises the following steps:
s1, storing a certain amount of boiler scale through a large-scale recovery mode; taking 1000-1500 parts of boiler scale, carrying out pretreatment on the selected boiler scale, including screening and drying treatment, crushing the boiler scale into granules of 3-5cm, and putting the granules into ultrafine crushing equipment until the granules are ultrafine crushed into particles with the size of 100 meshes to form boiler scale powder;
s2, putting the boiler scale powder in the S1 into a water storage tank which is prepared in advance, adding a certain amount of aqueous solution, and then stirring to form boiler scale powder slurry;
s3, adding a certain amount of disodium calcium edetate (CaNa) into the slurry formed in the step S22EDTA), heavy metal ion cadmium Cd of disodium edetate calcium boiler scale powder slurry2＋Aluminum Al3＋As, As3＋Hg, Hg2＋Neutralizing to form a stable and soluble metal chelate, and including each metal ion into the chelate to form a stable compound with larger molecular weight, so that the metal ions are prevented from acting in subsequent chemical reactions, and the influence of heavy metal substances on human bodies is avoided;
s4, adding a certain amount of acid solution into the slurry reacted in the step S3, wherein the acid solution is Mg (OH)2、CaCO3And a small amount of MgCO3All the components are subjected to acidolysis to form a product solution after acidolysis; the acid solution is concentrated sulfuric acid H2SO4At this time, the main substance reaction formula of acidolysis is:
Mg(OH)2＋H2SO4=MgSO4＋2H2O
CaCO3＋H2SO4=CaSO4＋H2O
MgCO3＋H2SO4=MgSO4＋H2O＋CO2↑
s5, filtering the product solution subjected to the acidolysis reaction of S4 to obtain CaSO in the product solution4Filtered off to form MgSO containing only the stable metal chelate4A solution;
s6, MgSO (MgSO) as described in S54Adding a quantity of water to the solution to form MgSO in accordance with the preparation concentration of the magnesium trisilicate4A solution;
s7, respectively preparing a certain amount of sodium silicate solution and a certain amount of sodium hydroxide solution, standing the sodium silicate solution, fully settling the sodium silicate solution, and mixing the sodium silicate solution with the sodium hydroxide solution;
s8, adding a certain amount of MgSO 6 in the step S6 into a reaction kettle prepared in advance4Adding the mixed solution of sodium silicate and sodium hydroxide obtained in the step S7 into the solution, and stirring for reaction after the addition is finished;
s9, pumping the reaction liquid obtained in the step S8 into a plate frame of a plate-and-frame filter press prepared in advance, washing with purified water, pulping after the primary washing, pumping the pulp into the plate frame of a clean area, continuing the secondary washing, and discharging the pressed plate after the washing;
s10, sampling and controlling, and drying after the free alkali is qualified;
the plate-and-frame filter press in the step S9 comprises a frame (1), a slide rail (11), a control box (12), an oil cylinder (13) and an oil supply unit (14); one end of the rack (1) is fixedly connected with an oil supply unit (14), and the oil supply unit (14) is connected with a power supply through a control box (12) on the rack (1); one side of the frame (1) far away from the oil supply unit (14) is fixedly connected with a fixed plate (15) through a pair of slide rails (11); one side of the slide rail (11) close to the fixed plate (15) is connected with a shunting block (2) in a sliding manner, and the slide rail (11) at one side of the shunting block (2) far away from the fixed plate (15) is connected with a group of filter plates (3) in a sliding manner; a pressing plate (16) is connected to the sliding rail (11) on one side, close to the oil supply unit (14), of the filter plate (3) in a sliding mode, and the pressing plate (16) is driven by an oil cylinder (13) fixedly connected to the rack (1); the oil cylinder (13) is communicated with the oil supply unit (14) through a pipeline; a feed pipe (17) is fixedly connected to one side of the fixing plate (15) far away from the shunting block (2), and high-pressure reaction liquid flows into the shunting block (2) through the feed pipe (17); a cylindrical separation cavity (21) is arranged in the shunting block (2), and a funnel-shaped separation barrel (22) is rotatably connected in the separation cavity (21); a rotating shaft at the bottom of the separating cylinder (22) is fixedly connected with an output shaft of a motor (23) fixedly connected to the bottom of the shunting block (2); the feeding pipe (17) is communicated with the separation cavity (21) through a feeding hole (24) on the shunting block (2), and the height of the feeding hole (24) is higher than the upper edge of the separation cylinder (22); the separation cylinder (22) and the separation cavity (21) are divided into four chambers (26) through a group of partition plates (25) fixedly connected to the inner wall of the separation cavity (21), and each chamber (26) is communicated with the filter plate (3) through a respective communication pipe (27); the isolation plate (25) is connected with the separation cylinder (22) in a sliding and sealing manner; a group of filtering holes (28) are uniformly formed in the circumference of the separating cylinder (22) between the adjacent partition plates, and the diameters of the four groups of filtering holes (28) are sequentially increased from top to bottom; a groove (31) is formed in one side, which is adjacent to the filter plate (3), and filter cloth (32) is arranged in the groove (31); a group of water filtering grooves (33) are uniformly formed in the bottom of the groove (31), and the water filtering grooves (33) are communicated with a water collecting pipe (35) below the filter plate (3) through a collecting pipe (34); the collecting pipe (34) is connected with an air source through an air supply pipe (36) on the filter plate (3) by a valve; a first slurry supplementing hole (37), a second slurry supplementing hole (38), a third slurry supplementing hole (39) and a fourth slurry supplementing hole (310) are sequentially formed in the upper part of the filter plate (3); the filter plate (3) is divided into a group A, a group B, a group C and a group D in sequence from one side close to the flow distribution block (2); the first pulp supplementing hole (37) is communicated with a groove (31) of the group A of filter plates (3), the second pulp supplementing hole (38) is communicated with a groove (31) of the group B of filter plates (3), the third pulp supplementing hole (39) is communicated with a groove (31) of the group C of filter plates (3), and the fourth pulp supplementing hole (310) is communicated with a groove (31) of the group D of filter plates (3); butterfly valves (311) for controlling the corresponding first slurry supplementing hole (37), second slurry supplementing hole (38), third slurry supplementing hole (39) and fourth slurry supplementing hole (310) are arranged on the filter plates (3) adjacent to the group A and the group B, the group B and the group C, and the group C and the group D; the first slurry supplementing hole (37), the second slurry supplementing hole (38), the third slurry supplementing hole (39) and the fourth slurry supplementing hole (310) are respectively communicated with the communicating pipe (27) at the corresponding position on the flow dividing block (2); the filter plate (3) is also provided with a group of water supply holes (312), and the water supply holes (312) are communicated with a pressure water source through a water pipe and a control valve; the water supply hole (312) is communicated with the groove (31); the water collecting pipe (35) is communicated with an air source through an air pipe and an electromagnetic valve;
when the device works, when material pressing and filtering are needed, firstly, the oil supply unit (14) is started through the control box (12), then the oil cylinder (13) is driven to press the filter plate (3) and the flow dividing block (2), then the reaction material liquid in the step S (8) is sent into the separating cylinder (22) in the separating cavity (21) through the feeding pipe (17) and the feeding hole (24) under high pressure, simultaneously, the starting motor (23) drives the separating cylinder (22) to rotate, under the action of centrifugal force, the rotating separating cylinder (22) separates particles with different sizes in the reaction material liquid due to different centrifugal force actions on the particles with different sizes, wherein the magnesium trisilicate particles in the reaction material liquid are increased from top to bottom in the separating cylinder (22), the particles with larger diameters in the reaction material liquid flow into the corresponding position cavity (26) from the filtering hole (28) close to the lower part of the separating cylinder (22), particles with smaller diameters in reaction liquid flow into a cavity (26) at a corresponding position from a filtering hole (28) close to the upper part of a separating cylinder (22) under the action of centrifugal force, the separated reaction liquid with different particle sizes flows into grooves (31) in corresponding groups of filter plates (3) through a first pulp supplementing hole (37), a second pulp supplementing hole (38), a third pulp supplementing hole (39) and a fourth pulp supplementing hole (310) respectively, the reaction liquid flows into a cavity formed by the grooves (31) and filter cloth (32) in adjacent filter plates (3), at the moment, the reaction liquid in a feed pipe (17) is continuously pressurized, so that water in the reaction between adjacent filter cloth (32) is extruded to form filter cakes, the extruded water flows into a water collecting pipe (35) after being collected by a collecting pipe (34) and then is recovered, an oil cylinder (13) is controlled by a control box (12) to retract, and purified water is introduced into a water supply hole (312) after the adjacent filter plates (3) are separated, flushing a filter cake formed in the groove (31), controlling the oil cylinder (13) to press the filter plate (3) through the control box (12), continuously pumping pressure reaction liquid into the groove (31) in the filter plate (3) to continuously extrude water, then withdrawing the oil cylinder (13), introducing purified water through the water supply hole (312) to flush the filter cake for the second time, finally opening the valve to supply air to the air supply pipe (36), and filling high-pressure air between the filter cloth (32) and the groove (31) through the collecting pipe (34) to enable the filter cake to be separated from the groove (31) after the filter cloth (32) expands, so that the filter cake falls;
because the diameters of the particles in the reaction feed liquid introduced into the group A, group B, group C and group D filter plates (3) are different, the diameters of the magnesium trisilicate particles in the filter cakes generated by the group A, group B, group C and group D filter plates (3) are different from each other, but the diameters of the magnesium trisilicate particles in the filter cakes in the same group of filter plates (3) are relatively uniform, and then, external personnel store the magnesium trisilicate generated by different groups in batches; due to the design of the mechanism, the magnesium trisilicate subjected to pressure filtration by the plate-and-frame filter press is uniform in diameter classification, and the condition that the diameters of a batch are not uniform is avoided;
meanwhile, a filter cake formed by particles with smaller diameters does not need to be ground, the subsequent grinding work is reduced, the production cost is saved, meanwhile, because the shunting block (2) is in close contact with the filter plate (3), the transportation distance of the reaction liquid after shunting is reduced, and the resistance of the reaction liquid on the pipeline wall in the flowing process is reduced, so that the pressure loss is reduced, the energy is saved, the purchase of a connecting pipe can be reduced, the equipment cost is reduced, meanwhile, the connecting link of the shunting block (2) and the filter plate (3) is reduced, and the possibility of leakage is reduced;
a cam (4) is fixedly connected to a rotating shaft at the bottom of the separating cylinder (22), and a cylinder (41) is arranged at the bottom of the separating cavity (21) and at a position corresponding to the cam (4); a first piston rod (42) in the cylinder (41) is in contact connection with the cam (4), and a spring is arranged in a rodless cavity of the cylinder (41); the butterfly valve (311) is a pneumatic valve, and the butterfly valve (311) is communicated with a rodless cavity of the cylinder (41) through a pipeline;
when the reaction liquid particles are uniform and flow division is not needed, high-pressure reaction liquid flows into a separating cylinder (22) in a separating cavity (21) through a feeding pipe (17) and a feeding hole (24), at the moment, a motor (23) is not started, the separating cylinder (22) does not rotate, the reaction liquid uniformly flows to filter plates (3) from each cavity (26) through a communicating pipe (27) to perform moisture filtration, at the moment, a cam (4) does not rotate, a cylinder (41) does not generate compressed gas, all butterfly valves (311) are opened under the action of the pressure of the reaction liquid after losing gas supply, the reaction liquid flows into all filter plates (3) to perform moisture filtration operation, when the reaction liquid with different particle diameters needs to be separated, the motor (23) is started to drive the cam (4) to rotate, and further the cylinder (41) generates the compressed gas to drive the butterfly valves (311) to close, namely, the reaction feed liquid with different particle diameters can be filtered in different areas;
one side of the filter plate (3) close to the groove (31) is uniformly provided with a group of horizontally arranged piston cylinders (5), and a second piston rod (51) is connected in the piston cylinders (5) in a sliding manner; one end, positioned outside the piston cylinder (5), of the second piston rod (51) faces the adjacent filter plate (3); a return spring (52) is arranged in a rodless cavity of the piston cylinder (5); a rod cavity of the piston cylinder (5) is communicated with the groove (31) through a pressurizing hole (53), and the pressurizing hole (53) penetrates through the filter cloth (32); a fastening cavity (54) is formed in the position, corresponding to the second piston rod (51), of the adjacent filter plate (3), and a clamping block (55) is rotatably connected in the fastening cavity (54); a clamping groove (56) is formed in the position, corresponding to the clamping block (55), of the second piston rod (51), and when the filter plate (3) is pressed tightly, the clamping block (55) rotates to clamp the clamping groove (56); the rotating shaft of the clamping block (55) is sleeved with a torsion spring for resetting the clamping block (55); a handle (57) is fixedly connected to one end of the rotating shaft of the clamping block (55) extending out of the filter plate (3);
after the adjacent filter plates (3) are tightly extruded, the other clamping grooves (56) of the second piston rod (51) are clamped by the clamping blocks (55), high-pressure reaction liquid is filled in the grooves (31), the reaction liquid enters the rodless cavity of the piston cylinder (5) through the pressurizing hole (53), the second piston rod (51) is pulled, the adjacent filter plates (3) are extruded more tightly, the probability that the reaction liquid leaks from gaps between the adjacent filter plates (3) is reduced, meanwhile, the reaction force between the squeezing pressure of the filtering press and the sealing pressure of the grooves (31) is reduced, the kinetic energy consumption is reduced, and the energy is saved;
the rod cavity of the piston cylinder (5) is communicated with the water supply hole (312) through a valve of the water spray hole (58), and the water spray hole (58) is used for spraying clean water to clean the inner wall of the piston cylinder (5); purified water in the water supply hole (312) is sprayed into the piston cylinder (5) through the water spray hole (58), so that reaction liquid participating in the piston cylinder (5) is cleaned, the reaction liquid is prevented from blocking the movement of the piston rod II (51), the condition that the piston cylinder (5) is inconvenient to use for the second time is avoided, and the condition that magnesium trisilicate is wasted because the magnesium trisilicate reaction liquid is retained in the piston cylinder and cannot fall off in the subsequent cleaning process is avoided;
the water spray holes (58) are communicated with air spray holes (59), and the air spray holes (59) are communicated with the collecting pipe (34) through pipelines and valves; the air injection holes (59) inject air into the water injection holes (58), and water is atomized and then injected out, so that the cleaning effect of the piston cylinder (5) is improved;
the jet holes (59) are used for jetting air to the water jet holes (58), so that water in the water jet holes (58) is atomized and then jetted out, the water consumption is saved, the water outlet speed is increased, the participating reaction material liquid in the piston cylinder (5) is further cleaned, and the reaction material liquid is prevented from blocking the motion of the second piston rod (51);
the water spray holes (58) are arranged along the tangential direction of the inner wall of the piston cylinder (5), and water flow sprayed out of the water spray holes (58) is sprayed out of the inner wall of the piston cylinder (5) to form wheel-spinning water flow, so that the cleaning dead angle in the piston cylinder (5) is reduced;
the water spray holes (58) arranged in the tangential direction of the inner wall of the piston cylinder (5) enable the sprayed water flow and water mist to form spiral water flow on the inner wall of the piston cylinder (5), so that the cleaning area and the cleaning efficiency are increased, the cleaning dead angle in the piston cylinder (5) is reduced, and the reaction liquid is further prevented from blocking the movement of the second piston rod (51);
the concentration of the sodium silicate solution is 15-25%, and MgSO is obtained in step S64The concentration of the solution is 15-20%, and the concentration of the sodium hydroxide is 15-20%;
molar ratio of feed, MgSO4: sodium silicate: sodium hydroxide = 1: (1.5-2.0): (2.5-3.0) and the reaction temperature is 10-60 ℃;
the pH control range of the controlled free alkali is 8-12.
2. The method for preparing and drying magnesium trisilicate according to claim 1, wherein: the drying mode can be vacuum drying, forced air drying, double cone drying and flash evaporation drying.
3. The method for preparing and drying magnesium trisilicate according to claim 2, wherein: the drying temperature of the vacuum drying, the forced air drying and the double-cone drying is 30-80 ℃, the air inlet temperature of the flash drying is 200-260 ℃, the air outlet temperature is 60-110 ℃, and the feeding frequency is 5-25 Hz.
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