CN105217643A - A kind of attapulgite clay prepares the method for δ-laminated crystal of sodium disilicate - Google Patents
A kind of attapulgite clay prepares the method for δ-laminated crystal of sodium disilicate Download PDFInfo
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- CN105217643A CN105217643A CN201410308099.1A CN201410308099A CN105217643A CN 105217643 A CN105217643 A CN 105217643A CN 201410308099 A CN201410308099 A CN 201410308099A CN 105217643 A CN105217643 A CN 105217643A
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- attapulgite clay
- sodium disilicate
- laminated crystal
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- recessed soil
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Abstract
A kind of attapulgite clay prepares the method for δ-laminated crystal of sodium disilicate, it is characterized in that: attapulgite clay mineral are after ore dressing, pulverizing, sieve to obtain attapulgite clay powder, under attapulgite clay powder being placed in high temperature, roasting destroys attapulgite clay structure, to add water and industrial sulphuric acid decomposes metal oxide in attapulgite clay, centrifugation, leaching liquid after solid-liquid separation is for the preparation of inorganic composite flocculant, and the throw out removed after a small amount of impurity of throw out bottommost is referred to as to activate recessed soil; Activate recessed soil and the reacted liquid of sodium hydroxide is placed in baking oven through concentrated, dry unbodied sodium disilicate; Amorphous sodium disilicate cools to obtain δ-laminated crystal of sodium disilicate in microwave oven after thermal treatment.
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 field of inorganic chemical engineering.
Background technology
Tripoly phosphate sodium STPP (STPP) is the washing auxiliary detergent that consumption is maximum, washing aid performance is superior up to now, but long-term a large amount of use of tripoly phosphate sodium STPP creates larger pollution to environment, has become the primary pollution source of body eutrophication.Countries in the world are constantly devoted to the research of the various substitute of STPP for many years, as the compound carbonate reported, various zeolite, Starso, Trisodium Citrate, nitrilotriacetic acid sodium (NTA), carboxylic methoxy succsinic acid trisodium (CMOS), polyacrylate, crystal layered sodium silicate etc.δ-laminated crystal of sodium disilicate is environment-friendly type hi-tech builder as substitute for phosphate.Due 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 with tripoly phosphate sodium STPP, thus the development research of δ-laminated crystal of sodium disilicate receives the extensive concern of people.
Summary of the invention
The object of the invention is to: provide a kind of attapulgite clay to prepare the method for δ-laminated crystal of sodium disilicate, the method with cheap mineral powder and attapulgite clay powder for main raw material, brilliant preparation high purity laminated crystal of sodium disilicate is turned with microwave, improve the added value of attapulgite clay on the one hand, reduce laminated crystal of sodium disilicate production cost, utilize the feature 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: attapulgite clay mineral are after ore dressing, pulverizing, sieve to obtain attapulgite clay powder, hereinafter referred to as recessed native powder, under attapulgite clay powder being placed in high temperature, roasting destroys attapulgite clay structure, to add water and industrial sulphuric acid decomposes metal oxide in attapulgite clay, centrifugation, the leaching liquid after solid-liquid separation is for the preparation of inorganic composite flocculant, and the throw out removed after a small amount of impurity of throw out bottommost is referred to as to activate recessed soil; Activate recessed soil and the reacted liquid of sodium hydroxide is placed in baking oven through concentrated, dry unbodied water glass; Unbodied water glass cools to obtain δ-laminated crystal of sodium disilicate in microwave oven after thermal treatment.
The method comprises following concrete steps:
(1) attapulgite clay mineral are through ore dressing, pulverize, sieve to obtain attapulgite clay powder, attapulgite clay powder is roasting 20 ~ 30min at 500 ~ 700 DEG C, be cooled to 110 DEG C to add water and be made into the recessed soil paste material that solid content is 15 ~ 25 quality %, drip industrial sulphuric acid in the slurry, sulfuric acid dosage is advisable with the pH value 1.0 ~ 2.5 maintaining final leaching liquid, hierarchy of control temperature 95 DEG C, under whipped state, leach 50 ~ 90min carry out solid-liquid separation, it is 4.5-6.0 centrifugation again that solid fraction is then washed with water to pH, the solid formation removed after being present in the trace impurity of solid phase bottommost is the recessed soil of activation, leaching liquid after separation is after 5: 3 through the ferro-aluminum ion ratio in ferric sulfate rearrange liquids, and being neutralized to pH value with sodium bicarbonate is 3.0, is polymerized 6h and prepares inorganic composite flocculant at temperature is 65 DEG C.
(2) recessed for activation soil is placed in flask, by SiO
2: Na
2the molar ratio weighing solid NaOH of O=1.9 ~ 2.1, the recessed soil of activation with through super-dry: water=1: the mass ratio of 2.5 ~ 3.5 adds water and is mixed with NaOH solution, NaOH solution is mixed with the recessed soil of activation, 1.5 ~ 2.0h is reacted under 90 DEG C ~ slight boiling condition, reacted liquid is placed in baking oven through concentrated, and at 120 ~ 180 DEG C, dry 40 ~ 60min obtains amorphous sodium disilicate;
(3) amorphous sodium disilicate is moved in microwave oven carry out turning brilliant process, its treating processes is thermal treatment 30 ~ 80min at 400 ~ 600 DEG C, then at the Temperature Treatment 30 ~ 60min of 720 ~ 780 DEG C, cool and obtain δ-laminated crystal of sodium disilicate product.
The technical indicator of δ-laminated crystal of sodium disilicate prepared by the present invention is: whiteness is 78 ~ 86%; The pH value of 0.1% aqueous solution: 10.5 ~ 11.5; With CaCO
3meter, 35 DEG C, 20min is in conjunction with calcium ion ability>=330mg/g (product); With MgCO
3meter, 35 DEG C, 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 cheap attapulgite clay mineral wealth to substitute chemical raw material production δ-laminated crystal of sodium disilicate in traditional method, improve the added value of attapulgite clay, reduce δ-laminated crystal of sodium disilicate raw materials for production cost; 2. utilize the waste liquid after acidleach to prepare inorganic composite flocculant, improve the utilization ratio of attapulgite clay mineral data; 3. microwave radiation body heat phase is utilized, overcome tradition to turn in crystal technique to be heated because material body is mutually non-homogeneous and cause asynchronous turn of crystalline substance and the defect of product performance instability that causes, meanwhile also shorten and turn the brilliant time from amorphous sodium disilicate to δ-laminated crystal of sodium disilicate.
Embodiment
Example 1
Recessed native powder 200g, containing SiO
2, Al
2o
3, Fe
2o
3be respectively 56.8%, 9.2% and 4.6%, roasting 20min at 620 DEG C, be cooled to 110 DEG C to add water and be mixed with the slurry that solid content is 20%, dripping concentration is in the slurry the industrial sulphuric acid of 92.5%, its pH value maintains 1.5, and hierarchy of control temperature is 95 DEG C, stir leach 60min under the state of trembling after centrifugation, it is 5.0 centrifugations again that solid fraction is washed with water to pH, removes after being sunken to a small amount of impurity of bottommost and must activate recessed soil;
Recessed for the activation of above-mentioned preparation soil is placed in flask, adds the aqueous solution 360ml containing 34.6g sodium hydroxide, be added to hot micro-boiling, at whipped state reaction 2h, reactant is placed in baking oven through concentrated, and at 140 DEG C, dry 55min obtains amorphous sodium disilicate.
The amorphous sodium disilicate of above-mentioned preparation reinstalled crucible and moves in microwave oven, thermal treatment 40min at 450 DEG C, cooling after then processing 40min at the temperature of 740 DEG C, obtaining 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 DEG C, 20min is 332mg/g (product) in conjunction with calcium ion ability; With MgCO
3meter, 35 DEG C, 20min is 453mg/g (product) in conjunction with magnesium ion ability.
Washings and leaching liquid merge, and with the ferro-aluminum ion ratio in ferric sulfate rearrange liquids, make [Al
3+]: [Fe
3+]=5: 3, then use NaHCO
3regulate pH to 3.0, be polymerized at temperature is 65 DEG C 6h inorganic composite flocculant product.
Example 2
Recessed native powder 100g, SiO
2content 52.1%, Al
2o
3content 8.4%, Fe
2o
3content 4.9%, at 650 DEG C after roasting 20min, be cooled to 110 DEG C and be mixed with water the slurry that solid content is 20%, be in the industrial sulphuric acid instillation slurry of 92.5% by concentration, maintain the pH value 2.0 of slurry, slurry is 95 DEG C in temperature and carries out speed change centrifugation after leaching 80min under stirring the state of trembling, and it is 5.5 that solid-phase material is washed with water to pH, removes a small amount of impurity in bottom and obtains active recessed soil.
Recessed for the activation of above-mentioned preparation soil is placed in flask, weighing sodium hydroxide 16.8g adds water 150ml, mix with the recessed soil of activation after sodium hydroxide dissolves, be heated to micro-boiling, at whipped state reaction 110min, reactant is placed in air dry oven, and at 150 DEG C, dry 45min obtains amorphous sodium disilicate.
The unbodied sodium disilicate of above-mentioned preparation is loaded crucible and moves in microwave oven, and thermal treatment 45min at 550 DEG C, cools after then processing 45min at the temperature of 760 DEG C, obtains 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 DEG C, 20min is 330mg/g (product) in conjunction with calcium ion ability; With MgCO
3meter, 35 DEG C, 20min is 451mg/g (product) in conjunction with magnesium ion ability.
Example 3
Recessed native powder 400g, SiO
2content 54.6%, Al
2o
3content 8.0%, Fe
2o
3content 3.5%, at 700 DEG C after roasting 30min, be cooled to 110 DEG C and be mixed with water the slurry that solid content is 25%, the pH to 2.5 of slurry is regulated with the industrial sulphuric acid that concentration is 92.5%, drip sulfuric acid as required in reaction process, make the pH value of slurry remain on 2.5, slurry is 95 DEG C and after leaching 1.5h under stirring the state of trembling in temperature, carry out speed change centrifugation again, being washed with water to pH is that bottom 6.0 removals, a small amount of impurity obtains active recessed soil.
Recessed for the activation of above-mentioned preparation soil is placed in flask, aqueous sodium hydroxide solution is mixed with sodium hydroxide 80g and 750ml water, pour in the reaction flask filling and activate recessed soil, the post-heating that is uniformly dispersed boils to micro-, at whipped state reaction 120min, reactant is placed in air dry oven, and at 180 DEG C, dry 60min obtains unbodied water glass.
The unbodied water glass of above-mentioned preparation is loaded crucible and moves in microwave oven, and thermal treatment 80min at 600 DEG C, then adjusts the temperature to 780 DEG C, cools, obtain δ-laminated crystal of sodium disilicate product 210g after continuing process 60min.
This product whiteness is 87%; 0.1% pH value of water solution is 11.3; With CaCO
3meter, 35 DEG C, 20min is 342mg/g (product) in conjunction with calcium ion ability; With MgCO
3meter, 35 DEG C, 20min is 465mg/g (product) in conjunction with magnesium ion ability.
Example 4
Recessed native powder 100g, SiO
2content 52.1%, Al
2o
3content 8.4%, Fe
2o
3content 4.9%, at 500 DEG C after roasting 20min, be cooled to 110 DEG C and be mixed with water the slurry that solid content is 15%, be in the industrial sulphuric acid instillation slurry of 92.5% by concentration, maintain the pH value 1.0 of slurry, slurry is 95 DEG C in temperature and carries out speed change centrifugation after leaching 50min under stirring the state of trembling, and it is that bottom 4.5 removals, a small amount of impurity obtains active recessed soil that solid-phase material is washed with water to pH.
The recessed soil of activation of above-mentioned preparation is placed in flask, and weighing sodium hydroxide 16.8g adds water 150ml, mixes after sodium hydroxide dissolves with the recessed soil of activation, be heated to 90 DEG C, at whipped state reaction 90min, reactant is placed in air dry oven, and at 120 DEG C, dry 40min obtains amorphous sodium disilicate.
The amorphous sodium disilicate of above-mentioned preparation is loaded crucible and moves in microwave oven, and thermal treatment 30min at 400 DEG C, cools after then processing 30min at the temperature of 720 DEG C, obtains 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 DEG C, 20min is 332mg/g (product) in conjunction with calcium ion ability, with MgCO
3meter, 35 DEG C, 20min is 450mg/g (product) in conjunction with magnesium ion ability.
Example 5
Recessed native powder 100g, SiO
2content 52.1%, Al
2o
3content 8.4%, Fe
2o
3content 4.9%, at 600 DEG C after roasting 25min, be cooled to 110 DEG C and be mixed with water the slurry that solid content is 20%, be in the industrial sulphuric acid instillation slurry of 92.5% by concentration, maintain the pH value 2.0 of slurry, slurry is 95 DEG C in temperature and carries out speed change centrifugation after leaching 70min under stirring the state of trembling, and it is that bottom 5.0 removals, a small amount of impurity obtains active recessed soil that solid-phase material is washed with water to pH.
Recessed for the activation of above-mentioned preparation soil is placed in flask, weighing sodium hydroxide 17.0g adds water 140ml, mix with the recessed soil of activation after sodium hydroxide dissolves, be heated to 100 DEG C, at whipped state reaction 100min, reactant is placed in air dry oven, and at 150 DEG C, dry 50min obtains amorphous sodium disilicate.
The amorphous sodium disilicate of above-mentioned preparation is loaded crucible and moves in microwave oven, and thermal treatment 45min at 500 DEG C, cools after then processing 50min at the temperature of 750 DEG C, obtains 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 DEG C, 20min is 336mg/g (product) in conjunction with calcium ion ability, with MgCO
3meter, 35 DEG C, 20min is 454mg/g (product) in conjunction with magnesium ion ability.
Claims (3)
1. an attapulgite clay prepares the method for δ-laminated crystal of sodium disilicate, it is characterized in that: attapulgite clay mineral are after ore dressing, pulverizing, sieve to obtain attapulgite clay powder, under attapulgite clay powder being placed in high temperature, roasting destroys attapulgite clay structure, to add water and industrial sulphuric acid decomposes metal oxide in attapulgite clay, centrifugation, leaching liquid after solid-liquid separation is for the preparation of inorganic composite flocculant, and the throw out removed after a small amount of impurity of throw out bottommost is referred to as to activate recessed soil; Activate recessed soil and the reacted liquid of sodium hydroxide is placed in baking oven through concentrated, dry unbodied sodium disilicate; Amorphous sodium disilicate cools to obtain δ-laminated crystal of sodium disilicate in microwave oven after thermal treatment.
2. attapulgite clay according to claim 1 prepares the method for δ-laminated crystal of sodium disilicate, it is characterized in that the method comprises following concrete steps: (1) attapulgite clay mineral are through ore dressing, pulverize, sieve to obtain attapulgite clay powder, attapulgite clay powder is roasting 20 ~ 30min at 500 ~ 700 DEG C, add water and be made into the recessed soil paste material that solid content is 15 ~ 25 quality %, drip industrial sulphuric acid in the slurry, sulfuric acid dosage is to maintain the pH value of final leaching liquid for 1.0 ~ 2.5, under whipped state, leach 50 ~ 90min carry out solid-liquid separation, it is 4.5-6.0 centrifugation that solid fraction is washed with water to pH, the solid formation removed after being present in the trace impurity of solid phase bottommost is the recessed soil of activation, (2) recessed for activation soil is placed in flask, by SiO
2: Na
2the molar ratio weighing solid NaOH of O=1.9 ~ 2.1, the recessed soil of activation with through super-dry: water=1: the mass ratio of 2.5 ~ 3.5 adds water and is mixed with NaOH solution, mixes NaOH solution with the recessed soil of activation, under 90 DEG C ~ slight boiling condition, reacts 1.5 ~ 2.0h, reacted liquid is placed in baking oven through concentrated, and at 120 ~ 180 DEG C, dry 40 ~ 60min obtains amorphous sodium disilicate, (3) amorphous sodium disilicate is moved in microwave oven carry out turning brilliant process, its treating processes is thermal treatment 30 ~ 80min at 400 ~ 600 DEG C, then after the Temperature Treatment 30 ~ 60min of 720 ~ 780 DEG C, cools and obtain δ-laminated crystal of sodium disilicate product.
3. attapulgite clay according to claim 2 prepares the method for δ-laminated crystal of sodium disilicate, it is characterized in that: the ferro-aluminum ion ratio that the leaching liquid after separation and washings merge in ferric sulfate rearrange liquids is 5: 3, being neutralized to pH value with sodium bicarbonate is 3.0, is polymerized 6h and prepares inorganic composite flocculant at temperature 65 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110229379A (en) * | 2019-07-02 | 2019-09-13 | 王豫园 | A kind of preparation method of sodium disilicate compound and its application in bearing material |
| CN110627077A (en) * | 2019-11-05 | 2019-12-31 | 中国科学院过程工程研究所 | Method for preparing sodium silicate by using sodium nitrate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6740300B1 (en) * | 1998-08-14 | 2004-05-25 | Korea Research Institute Of Chemical Technology | Method for manufacturing crystalline layered sodium disilicate |
| CN101007636A (en) * | 2007-01-13 | 2007-08-01 | 淮阴工学院 | Process for preparation of delta-layed crystalline sodium disilicate using attapulgite |
| CN103588212A (en) * | 2013-10-29 | 2014-02-19 | 清华大学 | Method for synthesizing delta-layered sodium disilicate by silicon tetrachloride |
-
2014
- 2014-07-01 CN CN201410308099.1A patent/CN105217643A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6740300B1 (en) * | 1998-08-14 | 2004-05-25 | Korea Research Institute Of Chemical Technology | Method for manufacturing crystalline layered sodium disilicate |
| CN101007636A (en) * | 2007-01-13 | 2007-08-01 | 淮阴工学院 | Process for preparation of delta-layed crystalline sodium disilicate using attapulgite |
| CN103588212A (en) * | 2013-10-29 | 2014-02-19 | 清华大学 | Method for synthesizing delta-layered sodium disilicate by silicon tetrachloride |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110229379A (en) * | 2019-07-02 | 2019-09-13 | 王豫园 | A kind of preparation method of sodium disilicate compound and its application in bearing material |
| CN110627077A (en) * | 2019-11-05 | 2019-12-31 | 中国科学院过程工程研究所 | Method for preparing sodium silicate by using sodium nitrate |
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