• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Novel alkali aluminum silicate particulates modified with and containing a chemically bound alkaline earth metal, and a method for producing same is disclosed. The alumino silicate pigments contain an alkaline earth metal, preferably calcium, magnesium or barium in addition to an alkali metal, such as sodium. In chemical composition, the pigments contain oxides of the alkaline earth metal, the alkali metal, aluminum and silicon and are distinguishable from co-precipitates. The pigments are prepared by introducing dilute solutions of an alkali silicate and an aluminum salt of a mineral acid into an agitated aqueous receiving medium containing an alkaline earth salt or hydroxide. The pH of the fuild reaction medium may be controlled to form finely divided precipitated particulates having improved properties and which may be used as pigments in paper, paint, rubber, inks, plastics and the like.
    公开号:SU786880A3
    申请号:SU721844620
    申请日:1972-11-03
    公开日:1980-12-07
    发明作者:Чарльз Фитон Роберт
    申请人:Дж. М. Губер Корпорейшн (Фирма)；
    IPC主号:
    专利说明:

    (54) METHOD FOR PRODUCING NATRIYSODERH ASCHEGO alkaline earth metal aluminosilicates invention relates to a technology for producing aluminosilicate containing in its composition the alkali and alkaline earth metals such as zeolites, when fit for use as adsorbents pigments and fillers such as paper, rubber compounds, plastics and paints. A known method of producing sodium aluminosilicates by reacting sodium silicate and aluminum sulfate when heated to 60 ° C is introduced into the working volume first with an aqueous solution of sodium silicate up to 50% of its amount, and then when it is fed simultaneously with a solution of aluminum sulfate heated to 52- 54-c and after the complete introduction of the latter with the supply of the rest of the sodium silicate to the reaction mixture. Formation: the precipitate is then pressed and dried with Cl3. A known method allows the production of sodium aluminosilicate used in papermaking. A known method of producing sodium alkaline earth metal silicate by reacting aqueous solutions of sodium silicate, an aluminum salt, such as sodium aluminosilicate, and a water-soluble alkaline earth metal salt, such as calcium or magnesium, in such a way that the aqueous solutions of said silicate and aluminum silicate are first mixed, followed by crystallization of the silicate and aluminum silicate. at 74-75 ° C, after which, this gel is mixed with the salt of an alkaline earth metal and the resulting mixture is kept at heating to a highlight. no crystallization of the product under cooling to room temperature. The precipitate formed in this way is separated, washed and dried. 2 The aluminosilicate obtained by this method has low sorption and pigment properties. In particular, it is characterized by the absorption of oil, amounting to no more than 106-112 cm- / OO g, and increased abrasion, characterized, for example, by an indicator of weight loss of the wire of 5.3-12.8 mg. The aim of the invention is to improve the adsorption and pigment properties of sodium alkaline earth metal silicate.
    The goal is achieved by obtaining sodium alkaline earth metal silicate by reacting aqueous solutions of sodium silicate, taken with a molar ratio of SiOg of 1-3.3: 1, aluminum salt and alkaline earth compound, so that the process is carried out by introducing aqueous solutions of silicate sodium and yoshümini salts in the form of separate streams separated from each other by the distance in the stirred aqueous solution of the salt or hydroxide of an alkaline earth metal — magnesium, barium or calcium with a concentration the last one in an amount that provides a metal content in a dry end product is 0.1-30%.
    At the same time, the introduction of a solution of sodium silicate into the working volume is possible by this method, first to a pH of 9.09, 9, followed by the continuation of its addition simultaneously with an aqueous solution of an aluminum salt,
    The difference of this method is that this interaction process is carried out with the introduction of aqueous solutions of sodium silicate and aluminum salts in the form of separate, spaced apart from each other, into the stirred aqueous solution of the alkaline earth metal compound at pH 8-12.
    The sodium silicate in this method is used with a molar ratio of Si: 0.2: NagO 1-3.3: 1.
    In addition, as the alkaline earth metal compound, its water-soluble salt or hydroxide is taken with the above-described concentration of an aqueous solution.
    In this case, sodium silicate is first introduced into an aqueous solution of a salt or alkaline earth metal hydroxide to pH 9.0–9.9, after which its introduction is continued simultaneously with an aqueous solution of an aluminum salt.
    The machine according to the present invention both bakes an improvement in the order of 18-20% of the adsorption properties of the sodium alkaline-earth metal-containing aluminosilicate obtained, as well as an improvement in its pigment properties, for example, in the best indicators of luminance and opacity of thin paper using the product obtained by the present invention. .
    The method of the invention is carried out as follows.
    Sodium silicate with a molar ratio of 1-3.3: 1 and an aluminum salt, preferably sulphate, is used as starting compounds for the production of the intended aluminosilicate, but it can be replaced by aluminum chloride or aluminum nitrate or aluminum-ammonium alum.
    As the alkaline earth metal compound, salt or magnesium hydroxide, calcium or barium is used.
    The preferred form of salts are water soluble salts, for example sulfates, carbonates, nitrates and chlorides, in particular calcium carbonate and magnesium sulphate.
    The ratio of oxides S i 0: ft in the reaction mixture is on the order of 2.5-24: 1 and 0.8-1.4: 1;
    In the process, the salts of aluminum and alkali metal silicate are dissolved at a very low level of concentration, and very 5 are vigorously stirred in the process of mixing them and co-introducing the alkaline earth metal compound into the solution.
    Diluted solutions of these 0 compounds with a concentration not exceeding the two molar concentration are introduced into the solution of an alkaline earth metal compound, amounting to about half the volume of the solutions introduced into it.
    Dilute silicate solutions and
    Aluminum salts are introduced into the initial working volume at points far from each other, for example, one can be introduced into the vortex funnel created by the paddle of the stirrer, and the other solution near the vessel wall.
    The addition of these solutions is started simultaneously or with the preliminary introduction of part of the silicate to a pH of about 8-12 with their subsequent introduction and after the introduction of the aluminum salt continues to introduce the silicate solution until the pH of the reaction mass equals 8-10.
    0 At the end of the reaction, precipitated
    The pigment is determined from a liquid by filtration or another separation method, for example, by centrifugation. The selected pigment is washed for
    5 removing water-soluble salts, e.g. water.
    The filter cake is dried before free water is removed from the pigment. Before its content is not more than 7-12%.
    0 Example, 5800 l of water are poured into a vessel with a capacity of 2840.0 l and L-580 kg of MgSO-yHgO is added, after which a stirrer is added, and the magnesium sulphate solution stirred in this manner is poured directly into a vortex formed by rotating blades of the vortex. A funnel of sodium silicate prepared from 2140 kg of sodium silicate Na2025S102 and L9000 l of water.
    60 Solutions of sodium silicate are thus introduced at a rate of 176 l / min for 16 minutes to a pH of the reaction mass of 9.9, after which the introduction of the silicate is continued simultaneously with aluminum sulphate at a rate of 95 liters / min for 35 minutes. As a result, reduction of the reaction mixture to a pH of 9.5. After the introduction of the entire amount of sodium silicate, the introduction of aluminum sulphate is continued for 15 minutes until the final pH of the reaction mass, and then the stirring of the reaction medium is continued for another 15 minutes.
    During this mixing of reagents, the temperature of the receiving medium is maintained at about
    At the end of the process, the precipitate formed is separated by filtration and washed thoroughly with water.
    The cake obtained by filtration is dried at and crushed on a hammer mill.
    The resulting material is finely sprayed particles with a diameter of less than 0.5 sec, and 97% of the particles have a diameter of less than 0 microns. The bulk density of the obtained product is 150 kg / m, the BET surface area is 97 m2 / g. Its chemical composition according to chemical analysis is 1.3 N3.0-1.0 A 1.0, 1.2 MdO-14.3 S i 4.3. EXAMPLE 2 The process is carried out analogously to example 1, but from the very beginning of the reaction and the precipitation process, solutions of aluminum sulphate and sodium silicate are simultaneously introduced and the pH of the reaction mixture is kept constant at 8, O by adjusting the input of the indicated reagents. at the end of the mixing period, which lasts 51 minutes, a diluted silicate solution is added to the mixture over about 3 minutes to a pH of 9.5. The resulting product is basically similar in properties to that described in the previous example. Froze The process is mainly carried out as in Example 1, but l-5600 g of water and 4-90 kg of calcium carbonate are loaded into the working container. The precipitated product is filtered, washed and dried, as in Example 1, and a pigment is obtained according to properties similar to that described above. The following table shows the properties of the aluminosilicate product A obtained according to the present invention using magnesium sulfate solution as the initial medium as compared to the known preparation of a similar product jB with the addition of MgSO4, simultaneously with sodium silicate, B with addition of MgS04 from the very beginning with silicate, and then during the final stage of addition simultaneously with the aluminum compound
    Surface area, m Intrusion of mercury,
    Bulk density, g / cm
    Compacted
    density,
    g / cm
    20.8 23.1 23.6
    Oil absorption, cMVlOO g
    130
    110 106
    Decrease attrition (loss in wire weight, mg)
    权利要求:
    Claims (4)
    [1]
    2,4 12,8 9,6 The above data indicate an increased adsorption capacity of the proposed product; and low abrasion characterizes it as a fine-grained pigment. The proposed pigment gives the paper an increased opacity and brightness of the order of 0.5-1.0% compared with the known aluminosilicate product. Claim 1. Instruction for producing sodium alkaline-earth aluminosilicate metal, including the interaction. aqueous solutions of sodium silicate. salts of aluminum and alkaline earth metal compounds, separation of the formed precipitate, washing it and drying, characterized in that in order to improve the adsorption and pigment properties of the target product, the interaction process is carried out with the introduction of aqueous solutions of sodium silicate and elumini salt in the form of separate, separated from each other at the distance of the streams, into the stirred aqueous solution of the alkaline earth metal compound and at a pH of 8-.12.
    [2]
    2. A method according to claim 1, characterized in that sodium silicate is used with a molar ratio of 1-3.3: 1.
    [3]
    3. Method POP1, characterized in that an alkaline earth metal compound is taken as its water-soluble salt, or hydroxide with a concentration in an aqueous
    7 7868808
    a solution providing content with an aqueous solution of an aluminum metal salt in a dry target product.
    0.1-30%. Sources of information,
    [4]
    4. The way pop.1 and 3, about tl and h a-taken into account in the examination
    y u u and with the fact that in the water plant-1. US patent No. 3582379,
    thief salt or alkali hydroxide-. cl. 106-288 V, 01.06.71.
    the grinding metal is first introduced into the system- 2. Patent OPr offen Iegungsschäfft
    sodium hydroxide to pH 9.0-9.9 after No. 1960361, cl. 12 32/26, 06.25.70
    which continues its introduction simultaneously (prototype).
    类似技术:
    公开号 | 公开日 | 专利标题
    SU786880A3|1980-12-07|Method of preparing sodium-containing alkaline-earth metal alumosilicate
    JP2939659B2|1999-08-25|Precipitated calcium carbonate
    US2848346A|1958-08-19|Production of zeolitic pigments
    JP2909371B2|1999-06-23|Waste material suspension treatment method
    US2739073A|1956-03-20|Silicate pigments
    US5342600A|1994-08-30|Precipitated calcium carbonate
    US3340003A|1967-09-05|Process for producing high purity alkaline earth compounds
    EP0480587B1|1994-11-17|Precipitated calcium carbonate
    US5445804A|1995-08-29|Process for the manufacture of pure amorphous silica from rocks
    JP4263864B2|2009-05-13|Novel composite for papermaking and method for synthesis
    US3197322A|1965-07-27|Preparation of calcium carbonate and the composition so made
    US2797978A|1957-07-02|Aluminum and magnesium hydroxy carbonate
    US3473890A|1969-10-21|Process for producing finely-divided,precipitated silicates and double silicates
    US4842772A|1989-06-27|Fire retardant pigment
    US2786758A|1957-03-26|Method of preparing siliceous pigment and method of preparing paper from such pigment
    US3915734A|1975-10-28|Modified precipitated alumino silicate pigments and method for preparing same
    USRE30568E|1981-04-07|Modified, precipitated alumino silicate pigments
    US2785991A|1957-03-19|Preparation of red oxide of iron
    CA1229331A|1987-11-17|Method of treating zeolite ores to remove discoloring impurities and improve its brightness and resultingfinely ground zeolitic product and coating materials,paper and coated paper containing same
    JPH0692632A|1994-04-05|Preparation of calcium sulfate
    US3592674A|1971-07-13|Method of preparing a calcium carbonate-magnesium hydroxide pigment and the pigment produced
    JP3902718B2|2007-04-11|Method for producing aragonite crystalline calcium carbonate
    US2595314A|1952-05-06|Process for producing magnesium hydroxide
    US2979380A|1961-04-11|Carbonate manufacture
    US2786777A|1957-03-26|Silica composition and production thereof
    同族专利:
    公开号 | 公开日
    NO135368C|1977-03-30|
    DK138112B|1978-07-17|
    FI56545C|1980-02-11|
    DE2253405C2|1982-10-21|
    US3798046A|1974-03-19|
    FR2158477B1|1976-04-23|
    NL7214752A|1973-05-08|
    IT970228B|1974-04-10|
    LU66405A1|1973-02-01|
    ES408286A1|1976-02-01|
    DE2253405A1|1974-06-27|
    FR2158477A1|1973-06-15|
    BE790801A|1973-04-30|
    SE380036B|1975-10-27|
    JPS5523205B2|1980-06-21|
    JPS4854000A|1973-07-28|
    FI56545B|1979-10-31|
    NO135368B|1976-12-20|
    CA981403A|1976-01-13|
    GB1414189A|1975-11-19|
    DK138112C|1978-12-27|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US2739073A|1950-09-06|1956-03-20|Huber Corp J M|Silicate pigments|
    US2848346A|1955-05-16|1958-08-19|Huber Corp J M|Production of zeolitic pigments|
    FR1577759A|1968-08-23|1969-08-08|
    DE1792585A1|1968-09-21|1971-11-25|Bayer Ag|Process for the continuous production of finely divided, amorphous sodium aluminum silicate fillers|
    BE790801A|1971-11-05|1973-04-30|Huber Corp J M|PROCESS FOR PREPARING MODIFIED SODIUM ALUMINOSILICATE PIGMENTS|USRE30568E|1971-11-05|1981-04-07|J. M. Huber Corporation|Modified, precipitated alumino silicate pigments|
    BE790801A|1971-11-05|1973-04-30|Huber Corp J M|PROCESS FOR PREPARING MODIFIED SODIUM ALUMINOSILICATE PIGMENTS|
    US3909286A|1971-11-05|1975-09-30|Huber Corp J M|Modified, precipitated alumino silicate pigments|
    US3928541A|1972-09-05|1975-12-23|Huber Corp J M|Amorphous precipitated siliceous pigments for cosmetic or dentrifrice use and methods for their production|
    US4213949A|1978-12-22|1980-07-22|E. I. Du Pont De Nemours And Company|Process of preparing particulate poly|
    US4213950A|1978-12-22|1980-07-22|E. I. Du Pont De Nemours And Company|Process for preparing amorphous particulate poly|
    US4557916A|1984-10-22|1985-12-10|J. M. Huber Corporation|Synthetic calcium silicates and methods of preparation|
    US5219660A|1987-06-01|1993-06-15|Wason Satish K|Precipitated encapsulated paper pigments and methods|
    US5312485A|1988-08-05|1994-05-17|J. M. Huber Corporation|Precipitated encapsulated paper pigments and methods|
    FI100659B|1988-08-05|1998-01-30|Huber Corp J M|Paper pigment composite products and process for their manufacture|
    US5352287A|1988-08-05|1994-10-04|J. M. Huber Corporation|Precipitated encapsulated paper pigments and methods|
    JPH0617217B2|1989-02-28|1994-03-09|水澤化学工業株式会社|Amorphous silica / alumina spherical particles and method for producing the same|
    CA2044644A1|1991-06-14|1992-12-15|Gerard Le Fevre|Method for the production of finely divided particulate siliceous material|
    FR2678259B1|1991-06-26|1993-11-05|Rhone Poulenc Chimie|NOVEL PRECIPITATED SILICA IN THE FORM OF GRANULES OR POWDERS, METHODS OF SYNTHESIS AND USE FOR REINFORCING ELASTOMERS.|
    US5575950A|1994-12-06|1996-11-19|J. M. Huber Corporation|Silicate defoaming composition and methods|
    US6127471A|1995-06-07|2000-10-03|Carchalk, Inc.|Coating system composition|
    US20030094253A1|2001-06-19|2003-05-22|Torras Joseph H.|Sodium silicate treatment for printing papers|
    FR2957914B1|2010-03-25|2015-05-15|Rhodia Operations|NOVEL PROCESS FOR PREPARING PRECIPITATED SILICES CONTAINING ALUMINUM|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US19802271A| true| 1971-11-05|1971-11-05|
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