CN102660158A - Dolomite/attapulgite composition and preparation method thereof - Google Patents
Dolomite/attapulgite composition and preparation method thereof Download PDFInfo
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- CN102660158A CN102660158A CN2012101048437A CN201210104843A CN102660158A CN 102660158 A CN102660158 A CN 102660158A CN 2012101048437 A CN2012101048437 A CN 2012101048437A CN 201210104843 A CN201210104843 A CN 201210104843A CN 102660158 A CN102660158 A CN 102660158A
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Abstract
The invention discloses a dolomite/attapulgite composition and a preparation method thereof. The preparation method comprises the following steps: depositing aluminum hydroxide and aluminum silicate on the surface of dolomite/attapulgite to obtain a dolomite/attapulgite composition; adding a dispersant and dolomite/attapulgite to deionized water, and dispersing 0.5-3h to obtain a dolomite/attapulgite slurry with the mass percentage of 5-30%; controlling the temperature of the slurry at 50-70DEG C, adjusting the pH of a system to 8-10 by an alkaline solution, adding a 1.6mol/L aqueous solution of sodium meta aluminate and a 0.2-0.8mol/L aqueous solution of an aluminum salt under stirring in a concurrent flow mode, and maintaining the pH of the system be unchanged; and heating the temperature of the slurry to 75-90DEG C, adding a 0.3-1.0mol/L aqueous solution of a silicate, adding a 0.2-0.8mol/L aqueous solution of an aluminum salt under stirring, continuously carrying out a temperature maintenance reaction for 0.5-3h, filtering, washing, drying, and crushing to obtain the dolomite/attapulgite composition. The preparation method which utilizes aluminum hydroxide and aluminum silicate to cooperatively brighten modified dolomite/attapulgite has the advantages of simplicity and easy implementation and mild conditions, and is suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of rhombspar/attapulgite composition and method of making the same, be specifically related to a kind ofly, belong to nonmetalliferous ore deep processing field with white lake and pure aluminium silicate modified synergic and the method that brightens rhombspar/attapulgite.
Background technology
A large amount of rhombspars is contained in the attapulgite clay mineral deposit, area in Soviet Union Anhui, and rhombspar/attapulgite is one of important ore type of this mine belt.Owing to this kind ore have loosely organized, particle diameter is little and be easy to the dispersive advantage has the potential using value.At present, the whiteness of rhombspar/attapulgite is generally about 80, can only use as low-grade filler, and price is cheap, causes the resource serious waste.Therefore, in order to improve the use value of rhombspar/attapulgite, also need further to improve its whiteness.
Summary of the invention
In view of the existing problem of background technology, the objective of the invention is to: a kind of rhombspar/attapulgite composition and method of making the same is provided, obtains the rhombspar/attapulgite compsn of high whiteness through this preparation method.
Technical solution of the present invention is: deposit white lake and pure aluminium silicate respectively in rhombspar/attapulgite's surface; Utilize white lake and pure aluminium silicate synergic whitening modification dolomite/attapulgite; Obtain the rhombspar/attapulgite compsn of high whiteness; This rhombspar/attapulgite compsn is made up of rhombspar/attapulgite, white lake and pure aluminium silicate; The mass ratio of white lake and rhombspar/attapulgite is 0.3 ~ 0.6:1 in the compsn, and the mass ratio of pure aluminium silicate and rhombspar/attapulgite is 0.4 ~ 0.8:1.
This rhombspar/attapulgite preparation of compositions method comprises following characterization step:
The preparation of step 1, rhombspar/attapulgite slurry: in deionized water, add dispersion agent and rhombspar/attapulgite; The mass ratio of dispersion agent and rhombspar/attapulgite is 0.01 ~ 0.05:1; Dispersion treatment 0.5 ~ 3 hour makes the quality percentage composition and is rhombspar/attapulgite slurry of 5% ~ 30%;
Step 2, white lake coat: the rhombspar/attapulgite slurry temperature of step 1 gained is controlled at 50 ~ 70 ℃; Using the pH value of alkali lye regulation system is 8 ~ 10; Stir on the limit; Bian Bingliu adds the sodium metaaluminate aqueous solution of 0.4 ~ 1.6 mol and the aluminum saline solution of 0.2 ~ 0.8 mol, and the pH value of maintenance system is constant;
Step 3, pure aluminium silicate are handled: the temperature of step 2 gained slurry is risen to 75 ~ 90 ℃, add the aqueous silicate solution of 0.3 ~ 1.0 mol, stir on the limit; The limit adds the aluminum saline solution of 0.2 ~ 0.8 mol, after aluminum saline solution adds, continues insulated and stirred reaction 0.5 ~ 3 hour; Filter washing, drying; Pulverize, obtain via white lake and pure aluminium silicate modified synergic and the rhombspar/attapulgite compsn that brightens.
Wherein, the described dispersion agent of step 1 is a kind of in Sodium hexametaphosphate 99, trisodium phosphate, tripoly phosphate sodium STPP, ZX-I, the ammonium polyacrylate.
Wherein, the described dispersion treatment of step 1 is that ultra-sonic dispersion, sand milling disperse and a kind of in disperseing of high-shear emulsion machine.
Wherein, the described aluminium salt of step 2 and step 3 is a kind of in Tai-Ace S 150, aluminum nitrate and the aluminum chloride.
Wherein, The add-on of the described sodium metaaluminate aqueous solution of step 2 and aluminum saline solution is by the white lake quality that they complete reactions generated, and the mass ratio of white lake and rhombspar/attapulgite is 0.3 ~ 0.6:1 (white lake: rhombspar/attapulgite=0.3 ~ 0.6:1).
Wherein, the described alkali lye of step 2 is a kind of in aqueous sodium hydroxide solution, potassium hydroxide aqueous solution and the ammoniacal liquor.
Wherein, the described silicate of step 3 is a kind of in water glass and the potassium silicate.
Wherein, the consumption of described aqueous silicate solution of step 3 and aluminum saline solution is by the quality of pure aluminium silicate that they complete reactions generate, and the mass ratio of pure aluminium silicate and attapulgite is 0.4 ~ 0.8:1.
Advantage of the present invention is:
(1) utilizes white lake and pure aluminium silicate modified synergic and brighten rhombspar/attapulgite, can obtain the rhombspar/attapulgite compsn of high whiteness, significantly improved value-added content of product.
(2) because rhombspar/attapulgite compsn contains white lake, in macromolecular material, not only have the effect of filler reinforcement, and have fire retardation.
(3) the method for the invention step is simple, and reaction conditions is gentle, is fit to large-scale production.
Embodiment
Further specify technical solution of the present invention below in conjunction with specific embodiment and comparative example, these embodiment can not be interpreted as it is the restriction to technical scheme.The measurement of the whiteness in embodiment and the comparative example is to carry out according to GB/T5950-1996 " Method for measurement of whiteness of building materials and nonMetal mineral products ".
Embodiment 1:
(1) in the deionized water of 1895 grams, adding 5 gram Sodium hexametaphosphate 99s and 100 gram whiteness is rhombspar/attapulgite powder of 78; With ME100 type high shearing mixing emulsor at a high speed (7000 rev/mins) disperseed 3 hours, be mixed with the quality percentage composition and be rhombspar/attapulgite slurry of 5%;
(2) with the temperature regulation of the rhombspar/attapulgite slurry of step 1 gained and remain on 50 ℃; Use quality percentage composition is 8% aqueous sodium hydroxide solution; The pH value of regulation system is 10; Stir on one side, on one side in slurries and drip add 480 milliliters of the aluminum sulfate aqueous solutions of 240 milliliters of the sodium metaaluminate aqueous solution and 0.4 mol of 1.6 mol, pH is constant for dropping process maintenance system;
(3) temperature with step 2 gained slurry rises to 90 ℃, 709 milliliters of the sodium silicate solutions of elder generation's adding 0.6 mol, and stir on the limit; The limit adds 355 milliliters of the aluminum sulfate aqueous solutions of 0.4 mol, after aluminum sulfate aqueous solution adds, continues insulated and stirred reaction 0.5 hour; Filter, and remove soluble salt, drying with the deionized water repetitive scrubbing; Pulverize, obtain the rhombspar/attapulgite compsn that brightens via white lake and pure aluminium silicate modified synergic.The mass ratio of white lake and rhombspar/attapulgite is 0.6:1 in rhombspar/attapulgite compsn, and the mass ratio of pure aluminium silicate and rhombspar/attapulgite is 0.4:1, and whiteness is 91.
Embodiment 2:
(1) in the deionized water of 897 grams, adding 3 gram tripoly phosphate sodium STPPs and 100 gram whiteness is rhombspar/attapulgite powder of 78; With the intelligent ultrasonic cell disruptor ultra-sonic dispersion of JYD650 0.5 hour, be mixed with the quality percentage composition and be rhombspar/attapulgite slurry of 10%;
(2) with the temperature regulation of the rhombspar/attapulgite slurry of step 1 gained and remain on 70 ℃; Use quality percentage composition is 5% ammonia soln; The pH value of regulation system is 8; Stir on one side, on one side in slurries and drip add 240 milliliters of the aluminum chloride aqueous solutions of 240 milliliters of the sodium metaaluminate aqueous solution and 0.8 mol of 0.8 mol, pH is constant for dropping process maintenance system;
(3) temperature with step 2 gained slurry rises to 80 ℃, 2837 milliliters of the potassium silicate solutions of elder generation's adding 0.3 mol, and stir on the limit; The limit adds 709 milliliters of the aluminum chloride aqueous solutions of 0.8 mol, after aluminum chloride aqueous solution adds, continues insulated and stirred reaction 3 hours; Filter, and remove soluble salt, drying with the deionized water repetitive scrubbing; Pulverize, obtain the rhombspar/attapulgite compsn that brightens via white lake and pure aluminium silicate modified synergic.The mass ratio of white lake and rhombspar/attapulgite is 0.3:1 in rhombspar/attapulgite compsn, and the mass ratio of pure aluminium silicate and rhombspar/attapulgite is 0.8:1, and whiteness is 92.
Embodiment 3:
(1) in the deionized water of 697 grams, adding 3 gram ZX-Is and 300 gram whiteness is rhombspar/attapulgite powder of 78, with SK2 sand Mill sand milling dispersion 2 hours, is mixed with the quality percentage composition and is rhombspar/attapulgite slurry of 30%;
(2) with the temperature regulation of the rhombspar/attapulgite slurry of step 1 gained and remain on 60 ℃; Use quality percentage composition is 3% potassium hydroxide aqueous solution; The pH value of regulation system is 9; Stir on one side, on one side in slurries and drip add 4808 milliliters of the aluminum nitrate aqueous solutions of 2404 milliliters of the sodium metaaluminate aqueous solution and 0.2 mol of 0.4 mol, pH is constant for dropping process maintenance system;
(3) temperature with step 2 gained slurry rises to 75 ℃, 1915 milliliters of the sodium silicate solutions of elder generation's adding 1.0 mol, and stir on the limit; The limit adds 6383 milliliters of the aluminum nitrate aqueous solutions of 0.2 mol, after aluminum nitrate aqueous solution adds, continues insulated and stirred reaction 2 hours; Filter, and remove soluble salt, drying with the deionized water repetitive scrubbing; Pulverize, obtain rhombspar/attapulgite compsn of brightening via white lake and pure aluminium silicate modified synergic, the mass ratio of white lake and rhombspar/attapulgite is 0.5:1 in rhombspar/attapulgite compsn; The mass ratio of pure aluminium silicate and rhombspar/attapulgite is 0.6:1, and whiteness is 93.
Comparative example 1:
(1) in the deionized water of 1895 grams, adding 5 gram Sodium hexametaphosphate 99s and 100 gram whiteness is rhombspar/attapulgite powder of 78; With ME100 type high shearing mixing emulsor at a high speed (7000 rev/mins) disperseed 3 hours, be mixed with the quality percentage composition and be rhombspar/attapulgite slurry of 5%;
(2) with the temperature regulation of the rhombspar/attapulgite slurry of step 1 gained and remain on 50 ℃; Use quality percentage composition is 8% aqueous sodium hydroxide solution; The pH value of regulation system is 10; Stir on one side, on one side in slurries and drip add 480 milliliters of the aluminum sulfate aqueous solutions of 240 milliliters of the sodium metaaluminate aqueous solution and 0.4 mol of 1.6 mol, pH is constant for dropping process maintenance system;
(3) temperature with step 2 gained slurry continues to maintain 50 ℃, 709 milliliters of the sodium silicate solutions of elder generation's adding 0.6 mol, and stir on the limit; The limit adds 355 milliliters of the aluminum sulfate aqueous solutions of 0.4 mol, after aluminum sulfate aqueous solution adds, continues insulated and stirred reaction 0.5 hour; Filter, and remove soluble salt, drying with the deionized water repetitive scrubbing; Pulverize, obtain rhombspar/attapulgite products via white lake and pure aluminium silicate modified synergic.The mass ratio of white lake and rhombspar/attapulgite is 0.6:1 in the product, and the mass ratio of pure aluminium silicate and rhombspar/attapulgite is 0.4:1, and the whiteness that records product is 88.
Comparative example 2:
(1) in the deionized water of 1895 grams, adding 5 gram Sodium hexametaphosphate 99s and 100 gram whiteness is rhombspar/attapulgite powder of 78; With ME100 type high shearing mixing emulsor at a high speed (7000 rev/mins) disperseed 3 hours, be mixed with the quality percentage composition and be rhombspar/attapulgite slurry of 5%;
(2) with the temperature regulation of the rhombspar/attapulgite slurry of step 1 gained and remain on 50 ℃, using the quality percentage composition is 8% aqueous sodium hydroxide solution, and the pH value of regulation system is 10; Stir on one side, on one side in slurries and drip add 800 milliliters of the aluminum sulfate aqueous solutions of 400 milliliters of the sodium metaaluminate aqueous solution and 0.4 mol of 1.6 mol, pH is constant for dropping process maintenance system; After adding, continue insulated and stirred reaction 0.5 hour, filter; And remove soluble salt with the deionized water repetitive scrubbing; Drying is pulverized, and obtains the rhombspar/attapulgite products via the white lake modification.The mass ratio of white lake and rhombspar/attapulgite is 1:1 in the product, and the whiteness that records product is 85.
Comparative example 3:
(1) in the deionized water of 1895 grams, adding 5 gram Sodium hexametaphosphate 99s and 100 gram whiteness is rhombspar/attapulgite powder of 78; With ME100 type high shearing mixing emulsor at a high speed (7000 rev/mins) disperseed 3 hours, be mixed with the quality percentage composition and be rhombspar/attapulgite slurry of 5%;
(2) temperature with the rhombspar/attapulgite slurry of step 1 gained rises to 90 ℃, adds 1773 milliliters of the sodium silicate solutions of 0.6 mol earlier, and stir on the limit; The limit adds 887 milliliters of the aluminum sulfate aqueous solutions of 0.4 mol, after aluminum sulfate aqueous solution adds, continues insulated and stirred reaction 0.5 hour; Filter, and remove soluble salt, drying with the deionized water repetitive scrubbing; Pulverize, obtain rhombspar/attapulgite products via the pure aluminium silicate modification.The mass ratio of product mesosilicic acid aluminium and rhombspar/attapulgite is 1:1, and the whiteness that records product is 86.
Claims (9)
1. rhombspar/attapulgite compsn; It is characterized in that: deposit white lake and pure aluminium silicate respectively in rhombspar/attapulgite's surface; Utilize white lake and pure aluminium silicate synergic whitening modification dolomite/attapulgite; Obtain the rhombspar/attapulgite compsn of high whiteness; This rhombspar/attapulgite compsn is made up of rhombspar/attapulgite, white lake and pure aluminium silicate, and the mass ratio of white lake and rhombspar/attapulgite is 0.3 ~ 0.6:1 in the compsn, and the mass ratio of pure aluminium silicate and rhombspar/attapulgite is 0.4 ~ 0.8:1.
2. rhombspar/attapulgite preparation of compositions method is characterized in that this preparation method comprises following characterization step:
The preparation of step 1, rhombspar/attapulgite slurry: in deionized water, add dispersion agent and rhombspar/attapulgite; The mass ratio of dispersion agent and rhombspar/attapulgite is 0.01 ~ 0.05:1; Dispersion treatment 0.5 ~ 3 hour makes the quality percentage composition and is rhombspar/attapulgite slurry of 5% ~ 30%;
Step 2, white lake coat: the rhombspar/attapulgite slurry temperature of step 1 gained is controlled at 50 ~ 70 ℃; Using the pH value of alkali lye regulation system is 8 ~ 10; Stir on the limit; Bian Bingliu adds the sodium metaaluminate aqueous solution of 0.4 ~ 1.6 mol and the aluminum saline solution of 0.2 ~ 0.8 mol, and the pH value of maintenance system is constant;
Step 3, pure aluminium silicate are handled: the temperature of step 2 gained slurry is risen to 75 ~ 90 ℃, add the aqueous silicate solution of 0.3 ~ 1.0 mol, stir on the limit; The limit adds the aluminum saline solution of 0.2 ~ 0.8 mol, after aluminum saline solution adds, continues insulated and stirred reaction 0.5 ~ 3 hour; Filter washing, drying; Pulverize, obtain via white lake and pure aluminium silicate modified synergic and the rhombspar/attapulgite compsn that brightens.
3. rhombspar according to claim 2/attapulgite preparation of compositions method is characterized in that: wherein, the described dispersion agent of step 1 is a kind of in Sodium hexametaphosphate 99, trisodium phosphate, tripoly phosphate sodium STPP, ZX-I, the ammonium polyacrylate.
4. rhombspar according to claim 2/attapulgite preparation of compositions method is characterized in that: wherein, the described dispersion treatment of step 1 is that ultra-sonic dispersion, sand milling disperse and a kind of in disperseing of high-shear emulsion machine.
5. rhombspar according to claim 2/attapulgite preparation of compositions method is characterized in that: wherein, the described aluminium salt of step 2 and step 3 is a kind of in Tai-Ace S 150, aluminum nitrate and the aluminum chloride.
6. rhombspar according to claim 2/attapulgite preparation of compositions method; It is characterized in that: wherein; The add-on of the described sodium metaaluminate aqueous solution of step 2 and aluminum saline solution is by the white lake quality that they complete reactions generated, and the mass ratio of white lake and rhombspar/attapulgite is 0.3 ~ 0.6:1.
7. rhombspar according to claim 2/attapulgite preparation of compositions method is characterized in that: wherein, the described alkali lye of step 2 is a kind of in aqueous sodium hydroxide solution, potassium hydroxide aqueous solution and the ammoniacal liquor.
8. rhombspar according to claim 2/attapulgite preparation of compositions method is characterized in that: wherein, the described silicate of step 3 is a kind of in water glass and the potassium silicate.
9. rhombspar according to claim 2/attapulgite preparation of compositions method; It is characterized in that: wherein; The consumption of described aqueous silicate solution of step 3 and aluminum saline solution is by the quality of pure aluminium silicate that they complete reactions generate, and the mass ratio of pure aluminium silicate and attapulgite is 0.4 ~ 0.8:1.
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| CN105226255A (en) * | 2015-10-20 | 2016-01-06 | 四川科能锂电有限公司 | The preparation technology of nickel ion doped |
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| CN109328513A (en) * | 2018-09-26 | 2019-02-15 | 江苏省地质调查研究院 | A kind of method and device for uniformly sowing ecological restoration material |
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| CN105355901A (en) * | 2015-10-20 | 2016-02-24 | 四川科能锂电有限公司 | Preparation method of lithium nickel manganese oxide |
| CN105968414A (en) * | 2016-05-13 | 2016-09-28 | 江苏艾特克阻燃材料有限公司 | Attapulgite-synergetic hydroxide flame retardant |
| CN105968414B (en) * | 2016-05-13 | 2018-11-23 | 江苏艾特克阻燃材料有限公司 | A kind of fire retardant and its method of modifying, fire proofing and preparation method thereof |
| CN109328513A (en) * | 2018-09-26 | 2019-02-15 | 江苏省地质调查研究院 | A kind of method and device for uniformly sowing ecological restoration material |
| CN109328513B (en) * | 2018-09-26 | 2022-08-05 | 江苏省地质调查研究院 | Method and device for uniformly spreading environment repairing material |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 211700 Jiangsu Xuyi Huaian County concave soil science and Technology Park Patentee after: Huaian Hua Hongxin materials Limited by Share Ltd Address before: 211700 Jiangsu Xuyi Huaian County concave soil science and Technology Park Patentee before: Xuyi Huahong Mining Co.,Ltd. |