CS251987B1 - A method of preparing high-flowing bentonite - Google Patents

A method of preparing high-flowing bentonite Download PDF

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CS251987B1
CS251987B1 CS855310A CS531085A CS251987B1 CS 251987 B1 CS251987 B1 CS 251987B1 CS 855310 A CS855310 A CS 855310A CS 531085 A CS531085 A CS 531085A CS 251987 B1 CS251987 B1 CS 251987B1
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Czechoslovakia
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bentonite
water
acid
weight
swelling
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CS855310A
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Czech (cs)
Slovak (sk)
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CS531085A1 (en
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Blahoslav Cicel
Peter Komadel
Jan Hronsky
Frantisek Rendos
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Blahoslav Cicel
Peter Komadel
Jan Hronsky
Frantisek Rendos
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Priority to CS855310A priority Critical patent/CS251987B1/en
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Publication of CS251987B1 publication Critical patent/CS251987B1/en

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Abstract

Na suchý bentonit alebo pastu bentonitu alebo suspenziu bentonitu s vodou sa působí pri teplote 2 až 110 °C počas 1 až 180 minút kyselinou chlorovodíkovou alebo kyselinou sírovou alebo kyselinou dusičnou pri koncentrácii kyseliny v zmesi 0,5 až 35 percent hmot. Získaná tuhá fáza sa premýva vodou. V případe přípravy kyslých bentonitov sa vysuší, v případe přípravy neutrálnych alebo slabo alkalických bentonitov sa zmieša s 1 až 10 % hmot. uhličitanu sodného a vysuší sa pri teplote 15 až 120 °C. Vysokonapučiavý bentonit má použitie v chémii, v potravinárstve, farmacii, kozmetike, veterinárstve, pri výrobě tepelnoizolačných materiálov.Dry bentonite or bentonite paste or bentonite suspension with water is treated at a temperature of 2 to 110 °C for 1 to 180 minutes with hydrochloric acid or sulfuric acid or nitric acid at an acid concentration in the mixture of 0.5 to 35 percent by weight. The obtained solid phase is washed with water. In the case of the preparation of acidic bentonites, it is dried, in the case of the preparation of neutral or weakly alkaline bentonites, it is mixed with 1 to 10% by weight of sodium carbonate and dried at a temperature of 15 to 120 °C. Highly swelling bentonite is used in chemistry, food industry, pharmacy, cosmetics, veterinary medicine, and in the production of thermal insulation materials.

Description

251987251987

Vynález sa týká spdsobu přípravy vyso-konapučiavého bentonitu.The present invention relates to a process for the preparation of high-activity bentonite.

Bentonit, ktorého zložkou je minerálmontmorillonit, sa vyznačuje okrem inýchvlastností aj tvorbou stabilných objemnýchsedimentov vo vodě. Zlepšenie napučiavostí(bobtnavostí) prírodných bentonitov sa do-siahne natrifikáciou, t. j. prídavkom uhli-čitanu sodného. Vyššie hodnoty napučiavos-tí sa dosiahnu natrifikáciou pri použití vib-račného mletia a stabilizáciou uchovánímpri tlaku 0 až 100 Pa alebo pri teplotách—70 až 0 °C alebo pri relatívnej vlhkostipod 0,1 % (čs. AO č. 199 882).Bentonite, the component of which is mineral montmorillonite, is characterized by, among other things, the formation of stable bulk sediments in water. The improvement in swelling of the natural bentonites is achieved by natrification, i.e. by the addition of sodium carbonate. Higher swelling values are achieved by natrification using vibratory grinding and stabilization of pressure retention at 0 to 100 Pa or at temperatures of -70 to 0 ° C or relative humidity of 0.1% (MS AO No. 199 882).

Nevýhodou takto vyrobených vysokonapu-čiavých bentonitov je to, že výrobok si vy-soká napučiavosť uchovává iba pri týchtoskladovacích podmienkach.A disadvantage of the high-flowing bentonites thus produced is that the product retains high swelling capacity only under these storage conditions.

Uvedené nevýhody odstraňuje v podstat-nej miere sposob přípravy vysokonapučia-vého bentonitu pósobením anorganickýchkyselin podl'a vynálezu.The above drawbacks are substantially eliminated by the preparation of high-flowing bentonite by the action of the inorganic acids of the invention.

Predmetom vynálezu je teda sposob pří-pravy vysokonapučiavého bentonitu posobe-ním anorganických kyselin vyznačený tým,že sa na suchý bentonit alebo pastu bento-nitu alebo suspenziu bentonitu s vodou po-sobí pri teplote 2 až 110 °C počas 1 až 180minút kyselinou chlorovodíkovou alebo ky-selinou sírovou alebo kyselinou dusičnoutak, aby výsledná koncentrácia kyseliny vzmesi bola hmotnostně 0,5 až 35 %, a zís-kaná tuhá fáza sa premýva vodou, zmiešasa s 0 až 10 % hmot. uhličitanu sodného avysuší sa pri teplote 15 až 120 °C.Accordingly, the present invention provides a process for the preparation of high swelling bentonite by the inorganic acid displacement of bentonite or bentonite or bentonite suspension with water at 2 to 110 ° C for 1 to 180 minutes with hydrochloric acid or with sulfuric acid or nitric acid, so that the resulting acid concentration of the mixture is 0.5 to 35% by weight, and the solid obtained is washed with water, mixed with 0 to 10% by weight. sodium carbonate and dried at 15 to 120 ° C.

Uvedený sposob přípravy vysokonapučia-vých bentonitov má výhodu, že produkt mávysoká napučiavosť a vysoká tixotropiu,ktoré si uchovává dlhý čas aj bez špeciál-nych skladovacích podmienok. Ďalšou vý-hodou je, že produkt mOže byť, podlá pří-davku uhličitanu sodného pri jeho príprave,kyslý, neutrálny alebo slabo alkalický.Příklad 1 152 g bentonitu (lokalita Jelšový Potok)s obsahom 34,2 % hmot. vody sa zmieša s348 g vody a dokladné sa premieša vrtulo-vým miešadlom. Suspenzia sa zahřeje nateplotu 90 °C a přidá sa 400 g hmotnostně35 %-né kyseliny chlorovodíkovej predhria-tej na teplotu 90 °C. Zmes sa nechá reago-vat 120 minát pri teplote 90 PC. Po ochladenía premytí třikrát 1 kg vody sa tuhá fázaoddělená filtráciou suší pri teplote 105 °C,zomelie sa na jemnost zrn pod 0,1 mm a sta-noví sa napučiavosť (bobtnavosť) podláČeskoslovenského liekopisu 3, zvázok II,Avicenum, Praha 1970 (ČSL-3): 2,0 g ben-tonitu nasýpa sa po malých častiach do100 cm3 vody v odmernom válci tak, že ďal-šia časť sa prisype až vtedy, keď predchá-dzajáca časť klesla ku dnu.^Po dvoch hodi-nách od začiatku nasýpania sa odčítá objemsuspenzie bentonitu vo vodě. Bentonit na-bobtnal na objem 82 cm3. Příklad 2 60 g bentonitu s obsahom 5,5 % hmot.vody a 10,4 % hmot. oxidu železitého sazmieša s 1140 g vody a dokladné sa pre-mieša. Suspenzia sa ohřeje na teplotu 50 °Ca přidá sa do nej 74 g hmotnostně 96 °/o-nejkyseliny sírovej. Zmes sa nechá reagovat 5minát pri teplote 50 °C. Po ochladení a pre-mytí třikrát 1 kg vody sa oddělí filtrácioutuhá fáza, zmieša sa s 3 g uhličitanu sod-ného, nechá sa 10 minát reagovat, vysuší sapri teplote 30 °C a zomelie sa na jemnostzfn pod 0,1 mm. Napučiavosť podlá CSL-3bola 48 cm3. Příklad 3 3 kg bentonitu (Maďarská ludová repub-lika) s obsahom 14,7 % hmot. vody sa zmie-ša v miesidle s 3 120 g vody. K získanejpaste sa přidá 1 060 g hmotnostně 96 %-nejkyseliny sírovej a pri trvalom premiešavanísa zmes nechá reagovat 40 minát pri tep-lote 25 °C. Potom sa pasta zriedl pridavKom10 kg vody, dekantuje a premýva sa eštedvakrát 10 kg vody. K premytej paste sa při-dá 216 g uhličitanu sodného, zmes sa pre-mieša a suší pri teplote 80 °C. Vysušenýprodukt sa zomelie na jemnost zrn pod 0,1milimeter. Napučiavosť podlá CSL-3 bola75 cm3. Příklad 4 1000 g plaveného bentonitu (lokalita Jel-šový Potok) s obsahom 14,2 % hmot. vodysa vsype do 5 kg hmotnostně 16 %-nej ky-seliny dusičnej predhriatej na teplotu 96 °C.Zmes sa nechá pri teplote 96 °C reagovat180 minát. Potom sa schladí prídavkom 5 kgvody a filtruje sa. Získaná pasta sa premý-va trikrát vždy s 5 kg vody. Do produktu poposlednom premytí sa přidá 17 g uhličitanusodného, zmes sa 15 minát premiešava, vy-suší sa pri teplote 105 °C a zomelie sa najemnost zrn pod 0,1 mm. Napučiavosť podláČSL-3 bola 87 cm3. Příklad 5 120 g bentonitu (Maďarská ludová repub-lika) s obsahom 14,7 % hmot. vody sa zmie-ša s 2 kg vody a suspenzia sa ohřeje na tep-lotu 96 °C. K suspenzii sa přidá 3 kg hmot-nostně 35 %-nej kyseliny chlorovodíkovejpredhriatej na teplotu 96 °C. Zmes sa necháreagovat 15 minát, schladí sa a premýva satrikrát 2 kg vody. Po premytí sa do pastypřidá 6 g uhličitanu sodného, zmes sa zho-mogenizuje, usuší sa pri teplote 60 °C a zo-melie sa na jemnost zfn pod 0,2 mm. Napu-čiavosť podlá ČSL-3 bola 80 cm3. Příklad 6Said method of preparing high-flowing bentonites has the advantage that the product has a high swelling capacity and high thixotropy, which is maintained for a long time even without special storage conditions. Another advantage is that the product may be acidic, neutral or weakly alkaline in the preparation of sodium carbonate. Example 1 152 g of bentonite (locality Jelšový Potok) with a content of 34.2% by weight. water is mixed with 348 g of water and mixed well with a propeller stirrer. The suspension is heated to 90 ° C and 400 g of 35 wt% hydrochloric acid preheated to 90 ° C are added. The mixture was allowed to react for 120 min at 90 ° C. After cooling and washing three times with 1 kg of water, the solid phase separated by filtration is dried at 105 ° C, milled to a grain size below 0.1 mm and swelling (Czechoslovakia Pharmacopoeia 3), II, Avicenum, Prague 1970 (CSL). -3): 2.0 g of ben-tonite is aspirated in small portions to 100 cm 3 of water in the metering cylinder so that the next portion is added only when the previous portion has dropped to the bottom. bentonite suspension in water is subtracted from the start of soaking. Bentonite swelled to a volume of 82 cm 3. Example 2 60 g of bentonite with a content of 5.5% w / w and 10.4% w / w. iron oxide is mixed with 1140 g of water and mixed well. The suspension is heated to 50 DEG C. and 74 g (96%) of sulfuric acid are added. The mixture was allowed to react for 5 min at 50 ° C. After cooling and washing three times with 1 kg of water, the filtration phase is separated off, mixed with 3 g of sodium carbonate, allowed to react for 10 minutes, dried at 30 DEG C. and milled to a pH below 0.1 mm. Swelling according to CSL-3bola was 48 cm 3. Example 3 3 kg bentonite (Hungarian human body) containing 14.7 wt. water is mixed in a stirrer with 3 120 g of water. To obtain the paste, 1060 g of 96% by weight sulfuric acid are added, and the mixture is left to react at 25 ° C for 40 minutes. Then the paste was diluted with 10 kg of water, decanted and washed twice with 10 kg of water. Sodium carbonate (216 g) was added to the washed paste, the mixture was stirred and dried at 80 ° C. The dried product is milled to a grain size of less than 0.1 millimeter. The swelling of CSL-3 was 75 cm 3. Example 4 1000 g of floated bentonite (locality Jelšový Potok) with a content of 14.2% by weight. the water is poured into 5 kg of 16% strength nitric acid preheated to 96 ° C. The mixture is allowed to react for 180 minutes at 96 ° C. It is then quenched by the addition of 5 kg of water and filtered. The paste obtained is washed three times with 5 kg of water each. 17 g of carbonate sodium is added to the final wash product, the mixture is stirred for 15 minutes, dried at 105 ° C, and the fineness of the grains is reduced to below 0.1 mm. The swelling of the sheet-3 was 87 cm 3. Example 5 120 g of bentonite (Hungarian human body) containing 14.7 wt. water is mixed with 2 kg of water and the suspension is heated to 96 ° C. To the suspension was added 3 kg of 35% hydrochloric acid preheated to 96 ° C. The mixture is not allowed to react for 15 minutes, cooled and washed twice with 2 kg of water. After washing, 6 g of sodium carbonate are added to the paste, the mixture is homogenized, dried at 60 ° C and ground to a fineness of less than 0.2 mm. The swelling of CSL-3 was 80 cm 3. Example 6

Postupuje sa rovnako ako v příklade 5 sThe procedure is as in Example 5 sec

Claims (1)

251 5 tým rozdielom, že sa použije hmotnostně 40 %-ná kyselina fosforečná namiesto hmot- nostně 35 °/o-nej kyseliny chlorovodíkové]. Napučiavosť pódia CSL-3 bola 15 cm3. 87 8 Vysokonapučiavý bentonit má široké po-užitie v chémii, potravinárstve, farmácii,kozmetike, veterinárstve, pri výrobě tepel-noizolačných materiálov. P R E D Μ E T Sposob přípravy vysokonapučiavého ben-tonitu posobením anorganických kyselinvyznačený tým, že sa na suchý bentonit ale-bo pastu bentonitu alebo suspenziu bento-nitu s vodou pósobí pri teplote 2 až 110 °Cpočas 1 až 180 minut kyselinou chlorovodí- YNÁLEZU kovou alebo kyselinou sírovou alebo kyseli-nou dusičnou pri koncentrácii kyseliny vzmesi hmotnostně 0,5 až 35 %, a získanátuhá fáza sa premýva vodou, zmieša na s 0až 10 % hmot. uhličitanu sodného a vysušísa pri teplote 15 až 120 °C.The difference is that 40% by weight phosphoric acid is used instead of 35% by weight of other hydrochloric acid]. The swelling of CSL-3 was 15 cm 3. 87 8 High-swelling bentonite has a wide use in chemistry, food, pharmacy, cosmetics, veterinary, thermal insulation materials. PREPARATION The process of preparing a high-swelling bentonite by inorganic acid treatment, characterized in that the bentonite or bentonite paste or bentonite suspension with water is treated at a temperature of 2 to 110 ° C for 1 to 180 minutes with hydrochloric acid or acid. with sulfuric acid or nitric acid at an acid concentration of 0.5 to 35% by weight, and the obtained phase is washed with water, mixed with 0 to 10% by weight. sodium carbonate and dried at 15 to 120 ° C.
CS855310A 1985-07-18 1985-07-18 A method of preparing high-flowing bentonite CS251987B1 (en)

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