LT4698B - Method for preparation of gypsum binding material - Google Patents
Method for preparation of gypsum binding material Download PDFInfo
- Publication number
- LT4698B LT4698B LT99-120A LT99120A LT4698B LT 4698 B LT4698 B LT 4698B LT 99120 A LT99120 A LT 99120A LT 4698 B LT4698 B LT 4698B
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- LT
- Lithuania
- Prior art keywords
- gypsum
- phosphogypsum
- binding material
- ratio
- binder
- Prior art date
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
- C04B11/26—Calcium sulfate cements strating from chemical gypsum; starting from phosphogypsum or from waste, e.g. purification products of smoke
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
Description
Išradimas priklauso neorganinių medžiagų gamybos technologijai, tai yra gipsinėms rišamosioms medžiagoms gauti iš fosfogipso (atliekos), gaunamo ekstrahuojant iš apatitų fosforo rūgštį sieros rūgštimi.The invention relates to a technology for the production of inorganic materials, that is to say gypsum binders obtained from phosphogypsum (waste) obtained by extraction of phosphoric acid with sulfuric acid from apatites.
Žinomas β-pushidračio gipso gavimo būdas iš fosfogipso neutralizavimo aktyviu kalcio oksidu, kur kietos masės ir vandens santykis esti 1:4, o pH kinta nuo (12,8-12,0) ir (12,06,5) per minutę (TSRS a.l. Nr. 1224287).A known method for preparing gypsum β-pushahydrate from neutralizing phosphogypsum with active calcium oxide is a solid to water ratio of 1: 4 and the pH varies between (12.8-12.0) and (12.066.5) per minute (USSR) al No. 1224287).
Žinomas gipso gamybos vandenilio iš fluorido rūgšties gamybos atliekos, rūgščių neutralizavimui naudojant lengvai pasiskirstančius rišamosios medžiagos masėje ferošlako lydalo miltelius (RU patentas Nr.2046097).Known waste from hydrofluoric acid production of gypsum by neutralizing acids using a ferroslag melt powder which is readily dispersed in a binder mass (RU Patent No. 2046097).
Artimiausias pagal esmę gipsinės rišamosios medžiagos gavimo būdas, susidedantis iš nuvandeninto fosfogipso priedo pridėjimo į fosfogipsą santykiu (0,6-1,8):1 bei masės maišymo (TSRS a.l. Nr. 1592281).The closest possible preparation of gypsum binder is the addition of dehydrated phosphogypsum additive to phosphogypsum in a ratio (0.6-1.8): 1 and mass mixing (USSR a.l. No. 1592281).
Tų technologijų trūkumas yra tas, kad visoms gipsinėms rišamosioms medžiagoms gauti sunaudojama daug energijos, todėl jų savikaina aukšta.The disadvantage of these technologies is that all gypsum binders use a lot of energy and therefore have a high cost.
Išradimo tikslas - iš fosfogipso atliekos, gaunamos ekstrahuojant fosforo rūgštį iš apatito veikiant jį sieros rūgštimi, gauti padidinto stiprumo rišamąsias medžiagas nenaudojant terminės dehidratacijos po fosfogipso neutralizacijos.The object of the present invention is to obtain high strength binders from the phosphogypsum waste obtained by extraction of phosphoric acid from apatite with sulfuric acid without the use of thermal dehydration after neutralization of the phosphogypsum.
Mechanine aktyvacija, trinant neutralizuotą šarminiais agentais pushidrati gipsą (basanitą), atpalaiduojamas kristalų karkasuose esantis nesurištas vanduo. Todėl kietėjančios struktūros formavimosi mechanizmas skiriasi nuo įprastinio pushidračio gipso kietėjimo. Pirminiame pushidračio gipso kietėjimo etape, struktūroje susidaro gipso karkasas dalyvaujant neutralizacijos agentams vienu atveju magnio hidroksidui, kitu atveju dalyvaujant portlandcemenčiui ir SiCty mikrodulkėms. Atsipalaidavus vandeniui iš kristalų karkaso, padidėja rišamųjų masių tankis ir jos įgauna papildomą stiprį bei padidėja atsparumas vandens poveikiui.Mechanical activation by the removal of alkaline agent-neutralized gypsum (basanite) releases the unbound water contained in the crystal skeletons. Therefore, the mechanism of formation of the hardening structure differs from the conventional hardening of solid hydrate gypsum. In the initial step of solidifying gypsum gypsum, the structure forms a gypsum skeleton in the presence of neutralizing agents in one case magnesium hydroxide, in the other case in the presence of Portland cement and SiCty micro dust. Relaxation of water from the crystal skeleton increases the binding mass density and adds strength and water resistance.
Išradimo tikslas pasiekiamas taip: į fosforo rūgšties ekstrakcijos procese šviežiai pasigaminusį pushidratį gipsą (basanitą) pridedama neutralizacijos agento - amorfinio magnio hidroksido gelio. Neutralizuotas mišinys termiškai neapdorojamas. Jo vandens-gipso santykis (V/G) su magnio hidroksidu iki normalios konsistencijos tešlos reguliuojama vandens pridėjimu j rišamąją masę. Kitu atveju, į šviežiai pasigaminusį fosfogipsą (basanitą) pridedama mišinio - neutralizacijos agento, susidedančio iš portlandcemenčio ir SiCh mikrodulkių - ferosilicio gamybos atliekos. Portlandcemenčio ir SiO: mikrodulkių santykis mišinyje yra 2:1, o fosfogipso ir neutralizacijos agento mišinio santykis 2,4:(0,7-1,3). Paruošto mišinio V/G taipogi reguliuojamas vandens priedu iki pasiekiama normali tešlos konsistencija.The object of the invention is achieved by the addition of a neutralizing agent, amorphous magnesium hydroxide gel, to freshly made push hydrate gypsum (basanite) in the process of extraction of phosphoric acid. The neutralized mixture is not heat treated. Its water-gypsum ratio (V / G) with magnesium hydroxide to a dough of normal consistency is controlled by the addition of water to the binder. Alternatively, the remainder of ferro-silicon from Portland cement and SiCh microparticles, a neutralization agent, is added to freshly made phosphogips (basanite). The ratio of Portland cement to SiO: micropowder in the mixture is 2: 1, and the ratio of phosphogypsum to neutralizing agent is 2.4: (0.7-1.3). The V / G of the prepared mixture is also adjusted with a water additive until the dough reaches its normal consistency.
Pirmu ir antru atvejais gauti mišiniai naudojami kaip įvairios paskirties rišamoji medžiaga, kaip antai aplinkos tvarkymo betoniniams gaminiams gaminti, grunto stabilizavimui kelių statyboje, monolitinėms grindims lieti ir kt.In the first and second cases, the resulting mixtures are used as a binder for various applications, such as for the production of concrete products for environmental management, for soil stabilization in road construction, for casting of monolithic floors, etc.
Fosfogipso ir priedų santykis turi būti toks kaip nurodyta šio patento apibrėžtyje, kadangi mažinant priedų kieki blogėja rišiklio rišamosios savybės. Didinant priedų kiekį rišiklio įtaka rišamosioms savybėms toliau nebegerėja, lieka tos pačios eilės, savikaina didėja.The ratio of phosphogypsum to additives must be as defined in this patent, since reducing the amount of additives decreases the binding properties of the binder. As the amount of additives increases, the influence of the binder on the binding properties no longer improves, remains in the same order, and the cost price increases.
Pagrindinė išeities žaliava gipsinio rišiklio yra šviežias fosfogipsas (basanitas), kuris naudojamas atvėsęs ne mažiau kaip iki 50°C temperatūros. Vidutinė fosfogipso cheminė sudėtis pateikiama 1 lentelėje.The basic raw material for the gypsum binder is fresh phosphogypsum (basanite), which is used after cooling to a temperature of at least 50 ° C. The average chemical composition of phosphogypsum is presented in Table 1.
lentelėtable
Bandymams naudojome:For testing we used:
Gelinį magnio hidroksidą pagal TS 5666739-30-96,Magnesium hydroxide gel according to TS 5666739-30-96,
Portlandeementį pagal 42.5 LST 1455.1996,Portland Element under 42.5 BS 1455.1996,
S1O2 mikrodulkes, importuojamas iš Lenkijos (ferosilicio gamybos atlieka). Jos gautos 3000°C temperatūroje (dalelių dydis 0,1-0,15μ).S1O2 Micro dust imported from Poland (Ferro-silicon waste). They were obtained at 3000 ° C (particle size 0.1-0.15µ).
Išradimą iliustruoja sekantys pavyzdžiai:The invention is illustrated by the following examples:
pavyzdys: Į >50°C temperatūros turinčią 3000 g fosfogipso (CaSChO^LLO) imtį, paimtą tiesiog nuo atliekų šalinimo konvejerio, pridedama 150 g 75% drėgmės turinčio magnio hidroksido gelio. Sausų medžiagų masės santykis 1:0,0125;Example: 150 g of 75% moisture content of magnesium hydroxide gel is added to a sample of 3000 g of phosphogypsum (CaSChO ^ LLO), taken directly from the waste disposal line, at a temperature of> 50 ° C. Dry solids weight ratio 1: 0.0125;
pavyzdys: Į 2400 g fosfogipso (CaSO4-0,5H2O) imtį pridedama 1000 g portlandcemenčio ir S1O2 mikro dulkių mišinio (sausų medžiagų santykis pridedame mišinyje 68% portlandcemencio ir 32% - S1O2 mikro dulkių). Fosfogipso (CaSO4-0,5H2O) ir priedo santykis 2,4:1. Paruoštų masių V/G reguliuojamas pridedant vandens iki normalios tešlos konsistencijos.Example 2: To a sample of 2400 g of phosphogypsum (CaSO 4 -0.5H 2 O) add 1000 g of a mixture of Portland cement and S1O2 micro dust (the dry matter ratio in the mixture is 68% Portland cement and 32% S1O2 micro dust). The ratio of phosphogypsum (CaSO 4 -0.5H 2 O) to additive is 2.4: 1. V / G of prepared masses is adjusted by adding water to normal dough consistency.
Abiem atvejais mišiniai maišomi mechaniškai aktyvuojant statgimėse po 45 min.In both cases, the mixtures were stirred by mechanical activation at a standstill after 45 min.
Tokiu būdu pagamintos rišiklių masės naudojamos liejimo būdu formuoti bandinėlius.The binder masses thus produced are used for molding test specimens.
Abiejų sudėčių bandiniai pažymėti atatinkamai numeriais 1-9 ir 10-18, sudėtys ir savybės pateiktos 2 lentelėje.Samples of both compositions are designated by numbers 1-9 and 10-18, respectively, and the compositions and properties are given in Table 2.
Kaip matome iš 2 lentelėje pateiktų duomenų, naudojant mechaninę aktyvaciją, gauta aukštos kokybės fosfogipsinė rišamoji medžiaga, iš kurios pagamintų bandinių fizinės-mechaninės savybės ženkliai viršija žinomus gamybos būdus. Gauta gipsinė rišamoji medžiaga yra atspari drėgmės poveikiui.As can be seen from the data in Table 2, mechanical activation produced a high-quality phosphogypsum binder, from which the physical-mechanical properties of the samples produced were significantly higher than those known in the art. The resulting gypsum binder is resistant to moisture.
Siūlomi rišikliai yra ekologiškai švarus, kadangi esamos fosfogipse fosforo rūgštis ir fluoras yra neutralizuojami šarminiais priedais.The proposed binders are ecologically clean, since phosphoric acid and fluorine are neutralized in the phosphogypsum with alkaline additives.
lentelėtable
- nuvandenintas fosfogipsas- Dehydrated phosphogypsum
Claims (3)
Priority Applications (1)
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LT99-120A LT4698B (en) | 1999-09-30 | 1999-09-30 | Method for preparation of gypsum binding material |
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LT99-120A LT4698B (en) | 1999-09-30 | 1999-09-30 | Method for preparation of gypsum binding material |
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LT4698B true LT4698B (en) | 2000-09-25 |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
LT5939B (en) | 2011-07-15 | 2013-05-27 | Vilniaus Gedimino technikos universitetas | Structural thermal insulation composite from local technogenic waste |
LT6739B (en) | 2018-10-04 | 2020-06-25 | Kauno technologijos universitetas | Method of preparation of high strength gypsum binder |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
SU1224287A1 (en) | 1982-12-27 | 1986-04-15 | Литовский Научно-Исследовательский Институт Строительства И Архитектуры | Method of producing beta-semihydrate of calcium sulfate |
SU1592281A1 (en) | 1988-06-20 | 1990-09-15 | Sumsk Kh Polt I | Method of producing gypsum binder from phospho-gypsum |
RU2046097C1 (en) | 1992-01-27 | 1995-10-20 | Анатолий Васильевич Левченко | Method of gypsum utilization from the waste of hydrofluoric acid or anhydrous hydrogen fluoride production |
-
1999
- 1999-09-30 LT LT99-120A patent/LT4698B/en not_active IP Right Cessation
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
SU1224287A1 (en) | 1982-12-27 | 1986-04-15 | Литовский Научно-Исследовательский Институт Строительства И Архитектуры | Method of producing beta-semihydrate of calcium sulfate |
SU1592281A1 (en) | 1988-06-20 | 1990-09-15 | Sumsk Kh Polt I | Method of producing gypsum binder from phospho-gypsum |
RU2046097C1 (en) | 1992-01-27 | 1995-10-20 | Анатолий Васильевич Левченко | Method of gypsum utilization from the waste of hydrofluoric acid or anhydrous hydrogen fluoride production |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
LT5939B (en) | 2011-07-15 | 2013-05-27 | Vilniaus Gedimino technikos universitetas | Structural thermal insulation composite from local technogenic waste |
LT6739B (en) | 2018-10-04 | 2020-06-25 | Kauno technologijos universitetas | Method of preparation of high strength gypsum binder |
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LT99120A (en) | 2000-06-26 |
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