CN101007636A - Process for preparation of delta-layed crystalline sodium disilicate using attapulgite - Google Patents
Process for preparation of delta-layed crystalline sodium disilicate using attapulgite Download PDFInfo
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- CN101007636A CN101007636A CNA2007100195550A CN200710019555A CN101007636A CN 101007636 A CN101007636 A CN 101007636A CN A2007100195550 A CNA2007100195550 A CN A2007100195550A CN 200710019555 A CN200710019555 A CN 200710019555A CN 101007636 A CN101007636 A CN 101007636A
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- sodium disilicate
- attapulgite clay
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- recessed soil
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Abstract
The invention discloses a making method of delta-layered crystallized sodium bisilicate through concavo-convex bar clay, which comprises the following steps: sintering concavo-convex bar clay under 500-700 deg.c for 20-30 min; cooling to 110 deg.c to allocate 15-25% slurry; dripping sulfuric acid with pH value to 1.0-2.5; controlling temperature to 95 deg.c; leaching for 50-90min; separating liquid from solid; washing to pH value at 4.5-6.0; centrifuging; separating to obtain active concave clay; weighing solid NaOH with the rate of SiO2 and Na2O at 1.9-2.1; allocating NaOH solution with cleaned concave clay and water at 1:2.5-3.5; adding NaOH solution into active concave clay to react 1.5-2.0 h under 90-microboiling condition; condensing liquid; placing condensate into baker; drying under 120-180 deg.c for 40-60 min; obtaining amorphous sodium bisilicate; transmitting amorphous sodium bisilicate into microwave oven; proceeding heat disposal under 400-600 deg.c for 30-80 min; disposing under 720-780 deg.c for 30-60 min; cooling to obtain the product.
Description
Technical field
The present invention relates to the method that attapulgite clay prepares δ-laminated crystal of sodium disilicate, belong to washing auxiliary detergent preparing technical field in the field of inorganic chemical engineering.
Background technology
Tripoly phosphate sodium STPP (STPP) is consumption maximum, the superior washing auxiliary detergent of washing aid performance up to now, but long-term a large amount of use of tripoly phosphate sodium STPP produced bigger pollution to environment, become the primary pollution source of body eutrophication.Countries in the world constantly are devoted to the research of the various substitutes of STPP for many years, as the compound carbonate of having reported, various zeolite, Starso, Trisodium Citrate, nitrilotriacetic acid sodium (NTA), carboxylic methoxy succsinic acid trisodium (CMOS), polyacrylate, crystallinity lamina sodium silicate etc.δ-laminated crystal of sodium disilicate is an environment-friendly type hi-tech builder as substitute for phosphate.Owing to δ-laminated crystal of sodium disilicate pH value surge capability, help the ability of washing, water demineralization and antiredeposition ability etc. comprehensively to help the ability of washing suitable, thereby the development research of δ-laminated crystal of sodium disilicate has been subjected to people's extensive concern with tripoly phosphate sodium STPP.
In recent years, the development research of δ-laminated crystal of sodium disilicate development is rapid, and relevant patent also is reported in media in succession.United States Patent (USP) 5236682 adopts quartz sand and sodium hydroxide to be mixed in proportion, and reaction synthetic water glass prepares laminated crystal of sodium disilicate through operations such as mode transfer, spraying drying and devitrification under the condition of high-temperature pressurizing; The CN1762804A patent is then directly with SiO
2With Na
2The mol ratio of O is the noncrystalline shape sodium disilicate of the aqueous solution of 1.8～2.3: 1 water glass with warm air spraying drying formation powdered, and the noncrystalline sodium disilicate of powdery is sent into the crystallization in the rotary kiln again, prepares the sodium disilicate of laminate structure through sintering; It is that 1.9～2.1 broken solid sodium silicates place devitrification equipment to carry out the method for devitrification Processing of Preparation laminated crystal of sodium disilicate that patent CN130130A has introduced modulus.The preparation method of the existing laminated crystal of sodium disilicate of analysis-by-synthesis, its raw materials for production are mainly the chemical raw material, production cost is higher, and noncrystalline sodium disilicate carries out under single high temperature to the brilliant process of the commentaries on classics of layered sodium disilicate, cause the laminated crystal of sodium disilicate purity of preparation not high, the performance shakiness, thereby restricted the promotion and application of laminated crystal of sodium disilicate in washing industry.
Summary of the invention
The objective of the invention is to: provide a kind of attapulgite clay to prepare the method for δ-laminated crystal of sodium disilicate, this method is that the attapulgite clay powder is a main raw material with cheap mineral powder, change brilliant preparation high purity stratiform crystalline sodium disilicate with microwave, improve the added value of attapulgite clay on the one hand, reduce the laminated crystal of sodium disilicate production cost, utilize the characteristics of microwave body heat phase on the other hand, improve the purity of δ-laminated crystal of sodium disilicate product, improve its comprehensive washing aid performance.
Technical solution of the present invention is: the attapulgite clay mineral are after ore dressing, pulverizing, sieve the attapulgite clay powder, hereinafter to be referred as recessed native powder, the attapulgite clay powder is placed roasting destruction attapulgite clay structure under the high temperature, add the metal oxide in water and the industrial sulphuric acid decomposition attapulgite clay, centrifugation, the leaching liquid after the solid-liquid separation is used to prepare inorganic composite flocculant, and the throw out behind a spot of impurity of removal throw out bottommost is referred to as active recessed soil; Active recessed soil places baking oven with the reacted liquid of sodium hydroxide through concentrating, dry must unbodied water glass; The thermal treatment in microwave oven of unbodied water glass cool off δ-laminated crystal of sodium disilicate.
This method comprises following concrete steps:
(1) the attapulgite clay mineral are through ore dressing, pulverize, sieve recessed native powder, recessed native powder is at 500～700 ℃ of following roasting 20～30min, being cooled to 110 ℃ adds water to be mixed with solid content (massfraction) is 15～25% recessed soil paste body, in slurry, drip industrial sulphuric acid, the sulfuric acid consumption is advisable with the pH value 1.0～2.5 of keeping final leaching liquid, 95 ℃ of hierarchy of control temperature, under whipped state, leach 50～90min and carry out solid-liquid separation, it is 4.5-6.0 centrifugation again that solid phase part then is washed with water to pH, removes solid formation behind the trace impurity that is present in the solid phase bottommost and promptly gets and activate recessed soil; After the ferro-aluminum ion ratio of leaching liquid after the separation in ferric sulfate adjustment liquid was 5: 3, being neutralized to the pH value with sodium bicarbonate was 3.0, is that 65 ℃ of following polymerization 6h prepare inorganic composite flocculant in temperature.
(2) will activate recessed soil and place flask, press SiO
2: Na
2The molar ratio weighing solid NaOH of O=1.9～2.1, to activate recessed soil through exsiccant: the mass ratio of water=1: 2.5～3.5 adds water and is mixed with NaOH solution, NaOH solution is mixed with active recessed soil, under 90 ℃～slight boiling condition, react 1.5～2.0h, reacted liquid is placed in the baking oven through concentrating, and gets amorphous sodium disilicate at 120～180 ℃ of down dry 40～60min;
(3) amorphous sodium disilicate is moved to change brilliant in the microwave oven and handle, its treating processes is at 400～600 ℃ of following thermal treatment 30～80min, and at Temperature Treatment 30～60min of 720～780 ℃, cooling promptly gets δ-laminated crystal of sodium disilicate product then.
The technical indicator of the δ-laminated crystal of sodium disilicate of the present invention's preparation is: whiteness is 78～86%; 0.1% pH value of aqueous solution: 10.5～11.5; With CaCO
3Meter, 35 ℃, 20min is in conjunction with calcium ion ability 〉=330mg/g (product); With MgCO
3Meter, 35 ℃, 20min is in conjunction with magnesium ion ability 〉=450mg/g (product); In Fe iron-holder≤0.02%.
The technical progress that the present invention obtains is: 1. utilize the chemical raw material production δ-laminated crystal of sodium disilicate in the alternative traditional method of cheap attapulgite clay mineral wealth, promote the added value of attapulgite clay, reduced δ-laminated crystal of sodium disilicate raw materials for production cost; 2. utilize the waste liquid after the acidleach to prepare inorganic composite flocculant, improved the utilization ratio of attapulgite clay mineral data; 3. utilize microwave radiation body heat phase, overcome the unsettled defective of product performance of being heated and causing asynchronous commentaries on classics crystalline substance to cause because of the material body is mutually non-homogeneous in traditional commentaries on classics crystal technique, meanwhile also shortened the brilliant time of commentaries on classics from amorphous sodium disilicate to δ-laminated crystal of sodium disilicate.
Specific implementation method
Example 1
Recessed native powder 200g contains SiO
2, Al
2O
3, Fe
2O
3Be respectively 56.8%, 9.2% and 4.6%, at 620 ℃ of following roasting 20min, being cooled to 110 ℃ adds water to be mixed with solid content is 20% slurry, dropping concentration is 92.5% industrial sulphuric acid in slurry, its pH value maintains 1.5, and hierarchy of control temperature is 95 ℃, is stirring centrifugation behind the leaching 60min under the state of trembling, it is 5.0 centrifugations again that solid phase partly is washed with water to pH, remove after the small amount of impurities be sunken to bottommost active recessed soil;
The active recessed soil of above-mentioned preparation is placed flask, and adding contains the aqueous solution 360ml of 34.6g sodium hydroxide, is added to little the boiling of heat, and at whipped state reaction 2h, reactant is placed in the baking oven through concentrating, and dry 55min gets amorphous sodium disilicate under 140 ℃.
The amorphous sodium disilicate of above-mentioned preparation reinstalled crucible and move in the microwave oven,, under 740 ℃ temperature, handle the 40min postcooling then at 450 ℃ of following thermal treatment 40min, δ-laminated crystal of sodium disilicate product 112g.
This product whiteness is 81%; 0.1% pH value of water solution is 11.2; With CaCO
3Meter, 35 ℃, 20min is 332mg/g (product) in conjunction with the calcium ion ability; With MgCO
3Meter, 35 ℃, 20min is a 453mg/g (product in conjunction with the magnesium ion ability.
Washings and leaching liquid merge, and the ferro-aluminum ion ratio with in the ferric sulfate adjustment liquid makes [Al
3+]: [Fe
3+]=5: 3 are used NaHCO again
3Regulate pH to 3.0, temperature be 65 ℃ of following polymerization 6h get final product the inorganic composite flocculant product.
Example 2
Recessed native powder 100g, SiO
2Content 52.1%, Al
2O
3Content 8.4%, Fe
2O
3Content 4.9%, behind 650 ℃ of following roasting 20min, being cooled to 110 ℃ of waters, to be mixed with solid content be 20% slurry, with concentration is that 92.5% industrial sulphuric acid splashes in the slurry, keep pH value of slurry 2.0, slurry is 95 ℃ and stirs under the state of trembling and carry out the speed change centrifugation behind the leaching 80min that in temperature it is 5.5 that solid-phase material is washed with water to pH, removes the bottom small amount of impurities and gets active recessed soil.
The active recessed soil of above-mentioned preparation is placed flask, weighing sodium hydroxide 16.8g adds water 150ml, treat to mix with the recessed soil of activity after the dissolution of sodium hydroxide, be heated to little boiling, at whipped state reaction 110min, reactant places air dry oven, and dry 45min gets amorphous sodium disilicate under 150 ℃.
With pack into crucible and moving in the microwave oven of the unbodied sodium disilicate of above-mentioned preparation, at 550 ℃ of following thermal treatment 45min, under 760 ℃ temperature, handle the 45min postcooling then, δ-laminated crystal of sodium disilicate product 54g.
This product whiteness is 78%; 0.1% pH value of water solution is 11.4; With CaCO
3Meter, 35 ℃, 20min is 330mg/g (product) in conjunction with the calcium ion ability; With MgCO
3Meter, 35 ℃, 20min is 451mg/g (product) in conjunction with the magnesium ion ability.
Example 3
Recessed native powder 400g, SiO
2Content 54.6%, Al
2O
3Content 8.0%, Fe
2O
3Content 3.5%, behind 700 ℃ of following roasting 30min, being cooled to 110 ℃ of waters, to be mixed with solid content be 25% slurry, with concentration is the pH to 2.5 that 92.5% industrial sulphuric acid is regulated slurry, drip sulfuric acid in the reaction process as required, make pH value of slurry remain on 2.5, slurry temperature be 95 ℃ and stir under the state of trembling leaching 1.5h after, carry out the speed change centrifugation again, being washed with water to pH is that 6.0 removal bottom small amount of impurities get active recessed soil.
The active recessed soil of above-mentioned preparation is placed flask, be mixed with aqueous sodium hydroxide solution with sodium hydroxide 80g and 750ml water, pour in the reaction flask that fills active recessed soil, be uniformly dispersed post-heating to little boiling, at whipped state reaction 120min, reactant places air dry oven, and dry 60min gets unbodied water glass under 180 ℃.
With pack into crucible and moving in the microwave oven of the unbodied water glass of above-mentioned preparation, at 600 ℃ of following thermal treatment 80min, adjust the temperature to 780 ℃ then, continue to handle the 60min postcooling, δ-laminated crystal of sodium disilicate product 210g.
This product whiteness is 87%; 0.1% pH value of water solution is 11.3; With CaCO
3Meter, 35 ℃, 20min is 342mg/g (product) in conjunction with the calcium ion ability; With MgCO
3Meter, 35 ℃, 20min is 465mg/g (product) in conjunction with the magnesium ion ability.
Example 4
Recessed native powder 100g, SiO
2Content 52.1%, Al
2O
3Content 8.4%, Fe
2O
3Content 4.9%, behind 500 ℃ of following roasting 20min, being cooled to 110 ℃ of waters, to be mixed with solid content be 15% slurry, with concentration is that 92.5% industrial sulphuric acid splashes in the slurry, keep pH value of slurry 1.0, slurry is 95 ℃ and stirs under the state of trembling and carry out the speed change centrifugation behind the leaching 50min that it is that 4.5 removal bottom small amount of impurities get active recessed soil that solid-phase material is washed with water to pH in temperature.
The active recessed soil of above-mentioned preparation places flask, and weighing sodium hydroxide 16.8g adds water 150ml, treats to mix with the recessed soil of activity after the dissolution of sodium hydroxide, be heated to 90 ℃, at whipped state reaction 90min, reactant places air dry oven, and dry 40min gets amorphous sodium disilicate under 120 ℃.
With pack into crucible and moving in the microwave oven of the amorphous sodium disilicate of above-mentioned preparation, at 400 ℃ of following thermal treatment 30min, under 720 ℃ temperature, handle the 30min postcooling then, δ-laminated crystal of sodium disilicate product 52g.
This product whiteness is 79%; 0.1% pH value of water solution is 11.2; With CaCO
3Meter, 35 ℃, 20min is 332mg/g (product) in conjunction with the calcium ion ability, with MgCO
3Meter, 35 ℃, 20min is 450mg/g (product) in conjunction with the magnesium ion ability.
Example 5
Recessed native powder 100g, SiO
2Content 52.1%, Al
2O
3Content 8.4%, Fe
2O
3Content 4.9%, behind 600 ℃ of following roasting 25min, being cooled to 110 ℃ of waters, to be mixed with solid content be 20% slurry, with concentration is that 92.5% industrial sulphuric acid splashes in the slurry, keep pH value of slurry 2.0, slurry is 95 ℃ and stirs under the state of trembling and carry out the speed change centrifugation behind the leaching 70min that it is that 5.0 removal bottom small amount of impurities get active recessed soil that solid-phase material is washed with water to pH in temperature.
The active recessed soil of above-mentioned preparation is placed flask, weighing sodium hydroxide 17.0g adds water 140ml, treat to mix with the recessed soil of activity after the dissolution of sodium hydroxide, be heated to 100 ℃, at whipped state reaction 100min, reactant places air dry oven, and dry 50min gets amorphous sodium disilicate under 150 ℃.
With pack into crucible and moving in the microwave oven of the amorphous sodium disilicate of above-mentioned preparation, at 500 ℃ of following thermal treatment 45min, under 750 ℃ temperature, handle the 50min postcooling then, δ-laminated crystal of sodium disilicate product 52.5g.
This product whiteness is 80%; 0.1% pH value of water solution is 11.5; With CaCO
3Meter, 35 ℃, 20min is 336mg/g (product) in conjunction with the calcium ion ability, with MgCO
3Meter, 35 ℃, 20min is 454mg/g (product) in conjunction with the magnesium ion ability.
Claims (3)
1. attapulgite clay prepares the method for δ-laminated crystal of sodium disilicate, it is characterized in that: the attapulgite clay mineral are after ore dressing, pulverizing, sieve the attapulgite clay powder, hereinafter to be referred as recessed native powder, the attapulgite clay powder is placed roasting destruction attapulgite clay structure under the high temperature, add the metal oxide in water and the industrial sulphuric acid decomposition attapulgite clay, centrifugation, leaching liquid after the solid-liquid separation is used to prepare inorganic composite flocculant, and the throw out behind a spot of impurity of removal throw out bottommost is referred to as active recessed soil; Active recessed soil places baking oven with the reacted liquid of sodium hydroxide through concentrating, dry must unbodied sodium disilicate; The thermal treatment in microwave oven of amorphous sodium disilicate cool off δ-laminated crystal of sodium disilicate.
2. attapulgite clay according to claim 1 prepares the method for δ-laminated crystal of sodium disilicate, it is characterized in that this method comprises following concrete steps:
(1) the attapulgite clay mineral through ore dressing, pulverize, sieve recessed native powder, recessed native powder is at 500～700 ℃ of following roasting 20～30min, adding water, to be mixed with the solid content mass ratio be 15～25% recessed soil paste body, in slurry, drip industrial sulphuric acid, the sulfuric acid consumption is 1.0～2.5 with the pH value of keeping final leaching liquid, under whipped state, leach 50～90min and carry out solid-liquid separation, it is the 4.5-6.0 centrifugation that solid phase partly is washed with water to pH, removes solid formation behind the trace impurity be present in the solid phase bottommost and promptly gets and activate recessed soil;
(2) will activate recessed soil and place flask, press SiO
2: Na
2The molar ratio weighing solid NaOH of O=1.9～2.1, to activate recessed soil through exsiccant: the mass ratio of water=1: 2.5～3.5 adds water and is mixed with NaOH solution, and NaOH solution is mixed with active recessed soil, reacts 1.5～2.0h under 90 ℃～slight boiling condition; Reacted liquid is placed in the baking oven through concentrating, and gets amorphous sodium disilicate at 120～180 ℃ of down dry 40～60min;
(3) amorphous sodium disilicate is moved to change brilliant in the microwave oven and handle, its treating processes is at 400～600 ℃ of following thermal treatment 30～80min, promptly gets δ-laminated crystal of sodium disilicate product at Temperature Treatment 30～60min postcooling of 720～780 ℃ then.
3. attapulgite clay according to claim 2 prepares the method for δ-laminated crystal of sodium disilicate, it is characterized in that: it is 5: 3 that leaching liquid after the separation and washings merge the ferro-aluminum ion ratio of adjusting in the liquid through ferric sulfate, being neutralized to the pH value with sodium bicarbonate is 3.0, and 65 ℃ of following polymerization 6h prepare inorganic composite flocculant in temperature.
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|---|---|---|---|
| CNB2007100195550A CN100457621C (en) | 2007-01-13 | 2007-01-13 | Process for preparation of delta-layed crystalline sodium disilicate using attapulgite |
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| Publication Number | Publication Date |
|---|---|
| CN101007636A true CN101007636A (en) | 2007-08-01 |
| CN100457621C CN100457621C (en) | 2009-02-04 |
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|---|---|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104129798A (en) * | 2014-06-25 | 2014-11-05 | 成都理工大学 | Method for preparing layered crystal sodium disilicate by using rice hull ash |
| CN105217643A (en) * | 2014-07-01 | 2016-01-06 | 蒋寿悟 | A kind of attapulgite clay prepares the method for δ-laminated crystal of sodium disilicate |
| CN106426546A (en) * | 2016-09-12 | 2017-02-22 | 淮阴工学院 | Integrated continuous production type clay dissociation-modification-drying method |
| CN109761241A (en) * | 2018-12-27 | 2019-05-17 | 济南大学 | A method of utilizing alkaline matter activated clays pore-creating |
| CN113772686A (en) * | 2021-10-22 | 2021-12-10 | 北京润捷浩达科技有限公司 | Method for preparing water glass and co-producing metal salt crystals by using silicon-rich clay |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2150607T3 (en) * | 1995-03-06 | 2000-12-01 | Clariant Gmbh | CRYSTALLINE STRATIFIED SODIUM SILICATE. |
| DE19537957A1 (en) * | 1995-10-12 | 1997-04-17 | Hoechst Ag | Process for the production of highly exchangeable sodium disilicate |
| CN1251349A (en) * | 1999-11-18 | 2000-04-26 | 殷宪国 | Method for preparing crystalline layered sodium silicate |
| CN1285504C (en) * | 2004-11-22 | 2006-11-22 | 河北科技大学 | Method for preparing laminated crystalline sodium disilicate by alta-mud |
-
2007
- 2007-01-13 CN CNB2007100195550A patent/CN100457621C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104129798A (en) * | 2014-06-25 | 2014-11-05 | 成都理工大学 | Method for preparing layered crystal sodium disilicate by using rice hull ash |
| CN105217643A (en) * | 2014-07-01 | 2016-01-06 | 蒋寿悟 | A kind of attapulgite clay prepares the method for δ-laminated crystal of sodium disilicate |
| CN106426546A (en) * | 2016-09-12 | 2017-02-22 | 淮阴工学院 | Integrated continuous production type clay dissociation-modification-drying method |
| CN109761241A (en) * | 2018-12-27 | 2019-05-17 | 济南大学 | A method of utilizing alkaline matter activated clays pore-creating |
| CN113772686A (en) * | 2021-10-22 | 2021-12-10 | 北京润捷浩达科技有限公司 | Method for preparing water glass and co-producing metal salt crystals by using silicon-rich clay |
| CN113772686B (en) * | 2021-10-22 | 2022-04-12 | 潘爱芳 | Method for preparing water glass and co-producing metal salt crystals by using silicon-rich clay |
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|---|---|
| CN100457621C (en) | 2009-02-04 |
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