CN110016243B - Dry preparation method of organic montmorillonite - Google Patents
Dry preparation method of organic montmorillonite Download PDFInfo
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- CN110016243B CN110016243B CN201910207586.1A CN201910207586A CN110016243B CN 110016243 B CN110016243 B CN 110016243B CN 201910207586 A CN201910207586 A CN 201910207586A CN 110016243 B CN110016243 B CN 110016243B
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- 229910017059 organic montmorillonite Inorganic materials 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims description 9
- 238000000034 method Methods 0.000 claims abstract description 29
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 9
- 239000011734 sodium Substances 0.000 claims abstract description 9
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 9
- 230000004048 modification Effects 0.000 claims abstract description 8
- 238000012986 modification Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 59
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 33
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 23
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 22
- 239000004254 Ammonium phosphate Substances 0.000 claims description 19
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 19
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 19
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000001488 sodium phosphate Substances 0.000 claims description 17
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 17
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 6
- 239000011575 calcium Substances 0.000 claims description 6
- 229910052791 calcium Inorganic materials 0.000 claims description 6
- 239000000839 emulsion Substances 0.000 claims description 6
- 229920003023 plastic Polymers 0.000 claims description 6
- 239000004033 plastic Substances 0.000 claims description 6
- 238000004945 emulsification Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000009775 high-speed stirring Methods 0.000 claims description 5
- 238000007670 refining Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- -1 organo montmorillonite Chemical compound 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 239000011229 interlayer Substances 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 238000011534 incubation Methods 0.000 abstract description 2
- 238000009830 intercalation Methods 0.000 description 4
- 230000002687 intercalation Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 3
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- VEUACKUBDLVUAC-UHFFFAOYSA-N [Na].[Ca] Chemical compound [Na].[Ca] VEUACKUBDLVUAC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
- C09C1/42—Clays
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
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- Chemical & Material Sciences (AREA)
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- Polymers & Plastics (AREA)
- Dispersion Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The method prepares the organic montmorillonite with high temperature resistance and larger interlayer spacing by surface coating, sodium-based conversion, surface modification, group conversion and incubation, simplifies the original process and increases the stripping property of the material.
Description
Technical Field
The invention relates to the technical field of montmorillonite treatment, in particular to a dry preparation method of organic montmorillonite.
Background
Montmorillonite (also known as montmorillonite or microcrystalline kaolinite) is a natural mineral of silicate, and is the main mineral component of bentonite ore. Containing Al2O3 16.54％；MgO 4.65％；SiO250.95 percent. Structural formula is (Al, Mg)2〔SiO10〕(OH)2·n H2And O. Monoclinic system, multi-site microcrystals, aggregates in the form of soil, spheres, etc. White, slightly grayish, yellowish, greenish, bluish when containing impurities, earthy luster or dull luster, and slippery feel. After adding water, it can expand several times its volume and become a paste. The volume of the product shrinks after heated dehydration. Has strong adsorption capacity and cation exchange performance, and is mainly produced in the weathering crust of volcanic tuff.
Montmorillonite (including calcium-based, sodium-calcium-based, magnesium-based montmorillonite) is peeled, dispersed, purified, modified, ultra-fine graded, and specially organically combined to obtain organic montmorillonite product with average wafer thickness less than 25nm, which can be used as bleaching agent and adsorbent filler, and is called universal material.
The montmorillonite is mainly used for adsorption and stripping, but the main stripping method is organic intercalation, but the temperature resistance of the montmorillonite is a great defect because the organic intercalation agent is mainly quaternary ammonium salt, and the surface organic of the montmorillonite is difficult to promote the material to be fundamentally changed.
Disclosure of Invention
The invention aims to overcome the defects of organic intercalation agents in the preparation of organic montmorillonite in the prior art, and provides a dry method preparation method of organic montmorillonite, which can obviously improve the surface stability and interlayer spacing of the obtained organic montmorillonite and simultaneously solve the problems of high-temperature discoloration and easy agglomeration.
The invention adopts the technical scheme that the dry preparation method of the organic montmorillonite comprises the following steps:
step 1, emulsification: taking montmorillonite, stirring in a stirring kettle, adding polyvinyl alcohol emulsion, and stirring for 20-30min to make the materials uniform;
step 2, sodium modification: gradually heating the uniform substance obtained in the step 1 to 60-80 ℃, adding a sodium phosphate solution, and stirring for 50-60 min;
and step 3, drying: continuously heating the mixture obtained in the step 2 to 100 ℃, and stirring for 3-5 hours until the product is dried;
step 4, crushing: taking out the dried product obtained in the step (3), and putting the dried product into a mechanical crusher for crushing until the preset fineness range is reached;
step 5, organizing and acidifying: adding a silane coupling agent into deionized water, stirring uniformly, adding ammonium phosphate, and continuously stirring uniformly to form a mixed solution of the silane coupling agent and the ammonium phosphate; putting the powder crushed in the step (4) into a high-speed stirring kettle, stirring at a high speed, adding the powder into the mixed solution of the silane coupling agent and the ammonium phosphate, stirring for 15min, adding acetic acid, and continuing stirring at a high speed for 30 min;
step 6, refining: and (5) taking the powder uniformly stirred in the step (5), putting the powder into a jet mill, grinding the powder to a preset fineness, adding the powder into a sealed plastic bag, and sealing and storing the bag for 7 days to obtain the organic montmorillonite prepared by the dry method.
The method prepares the organic montmorillonite with high temperature resistance and larger interlayer spacing through the processes of surface coating, sodium-based conversion, surface modification, group conversion, incubation and the like in the steps, simplifies the original preparation process and flow and increases the stripping property of the material.
Further, in the step 1, the montmorillonite is calcium-based montmorillonite, the mass ratio of the polyvinyl alcohol to the montmorillonite is 1 (500- > 1000), and the stirring speed is 80-150 r/min.
The polyvinyl alcohol can improve the viscosity of the montmorillonite and the binding capacity with a coupling agent in a subsequent step.
Further, in the step 2, the mass ratio of the sodium phosphate to the water in the sodium phosphate solution is as follows: 1, (10-50); the mass ratio of the addition amount of the sodium phosphate solution to the montmorillonite in the step 1 is 1: (80-200), the stirring speed is 200-400 r/min.
The sodium phosphate is strong base weak acid salt, and can perform sodium treatment on the montmorillonite to obtain sodium-treated montmorillonite.
Further, in the step 3, the stirring speed is 80-150 r/min, and the product drying means that the water content in the product is less than or equal to 10% by mass.
Further, the predetermined fineness range in the step 4 is 300-800 meshes.
Further, in the step 5, the silane coupling agent is one of KH560, KH580, KH791, KH792, KH901 and KH 902; the mass ratio of the silane coupling agent to the montmorillonite in the step 1 is 1 (100-); the mass ratio of the deionized water to the silane coupling agent is (5-10) to 1; the mass ratio of ammonium phosphate to the montmorillonite in the step 1 is as follows: 1 (200-500); the stirring speed is 600-1200 rpm.
Ammonium phosphate can replace sodium phosphate to accelerate the reaction of the hydrolytic silane coupling agent and the montmorillonite. Meanwhile, the organizing effect of the montmorillonite is ensured.
Furthermore, the mass ratio of the ammonium phosphate in the mixed liquid of the silane coupling agent and the ammonium phosphate is 8-15%.
Further, the predetermined fineness in the step 6 is 1500-3000 meshes.
Compared with the prior art, the invention has the advantages that:
1) the surface stability of the obtained organic montmorillonite is obviously improved by coating the silane coupling agent; the interlayer spacing of the obtained organic montmorillonite is obviously improved by using the reaction of polyvinyl alcohol and hydrolyzed silane
2) Compared with the traditional process, the method has the advantages that the method is high in feasibility and convenient to use, and compared with the traditional process, the method firstly uses a dry method for preparation, saves a large amount of water resources, and secondly, the dry method does not need drying treatment, uses a high-temperature-resistant coupling agent and phosphate for treatment, and does not agglomerate for the second time after coating.
3) The invention prepares the organic montmorillonite by using the dry method, and solves the problems of extrusion molding or deeper synthetic reaction color and easy color change in plastics due to the fact that the quaternary ammonium salt is not resistant to high temperature in the traditional quaternary ammonium salt intercalation method.
Detailed Description
The present invention will be described in further detail below with reference to specific embodiments in order to make the present invention better understood by those skilled in the art.
Example 1
A dry method for preparing organic montmorillonite comprises the following steps:
step 1, emulsification: dissolving 10g of polyvinyl alcohol into 50ml of solution, and uniformly stirring to form polyvinyl alcohol emulsion; 1000g of calcium-based montmorillonite is stirred in a stirring kettle, 10ml of polyvinyl alcohol emulsion is added, and the stirring is carried out for 25MIN at the speed of 100 r/MIN.
Step 2, sodium modification: dissolving 10g of sodium phosphate in 100ml of water to form a sodium phosphate solution; the stirred tank was gradually heated to 65 ℃ and 100ml of sodium phosphate solution was added and stirred at 200 rpm for 60 MIN.
And step 3, drying: heating to 100 deg.C, and stirring at 100 rpm/MIN for 5 hr until the water content is 8 wt%.
Step 4, crushing: taking out the dried product, and placing the dried product in a mechanical crusher for crushing to obtain the fineness of 300 meshes.
Step 5, organizing and acidifying: adding 10gKH560 silane coupling agent into 50ml deionized water, stirring uniformly, adding 5g ammonium phosphate into the solution, and continuing stirring until uniform; and (3) putting the powder obtained in the step (4) into a high-speed stirring kettle, stirring at a high speed, adding the powder into a mixed solution of a silane coupling agent and an ammonium phosphate solution, stirring for 15MIN, adding 3ml of acetic acid, and continuing stirring at a high speed for 30 MIN.
Step 6, refining: taking out the uniformly stirred powder, placing the powder in a jet mill for grinding to the fineness of 2500 meshes, adding the powder into a sealed plastic bag, and sealing and storing for 7 days to obtain the organic montmorillonite prepared by the dry method.
Through the steps, the dry-method organic montmorillonite is prepared.
Example 2
A dry method for preparing organic montmorillonite comprises the following steps:
step 1, emulsification: dissolving 10g of polyvinyl alcohol into 50ml of solution, and uniformly stirring; 1000g of calcium-based montmorillonite is stirred in a stirring kettle, 20ml of polyvinyl alcohol emulsion is added, and the stirring is carried out for 25MIN at the speed of 100 r/MIN.
Step 2, sodium modification: dissolving 20g sodium phosphate in 100ml water to obtain solution, gradually heating the stirring kettle to 65 deg.C, adding 100ml sodium phosphate solution, and stirring at 200 rpm/MIN for 60 MIN.
And step 3, drying: heating to 100 deg.C and stirring at 100 rpm for 5 hr until the water content is 8%.
Step 4, crushing: taking out the dried product, and placing the dried product in a mechanical crusher for crushing to obtain the fineness of 300 meshes.
Step 5, organizing and acidifying: adding 5gKH570 silane coupling agent into 40ml deionized water, stirring uniformly, adding 6g ammonium phosphate into the solution, and continuing stirring until uniform; and (3) putting the powder obtained in the step (3) into a high-speed stirring kettle, stirring at a high speed, adding the powder into a mixed solution of a silane coupling agent and an ammonium phosphate solution, stirring for 15MIN, adding 3ml of acetic acid, and continuing stirring at a high speed for 30 MIN.
Step 6, refining: taking out the uniformly stirred powder, placing the powder in a jet mill for grinding to the fineness of 2500 meshes, adding the powder into a sealed plastic bag, and sealing and storing for 7 days to obtain the organic montmorillonite prepared by the dry method.
Through the steps, the dry-method organic montmorillonite is prepared.
Example 3
A dry method for preparing organic montmorillonite comprises the following steps:
step 1, emulsification: dissolving 10g of polyvinyl alcohol into 50ml of solution, and uniformly stirring; 1000g of calcium-based montmorillonite is stirred in a stirring kettle, 15ml of polyvinyl alcohol emulsion is added, and the stirring is carried out for 25MIN at the speed of 100 r/MIN.
Step 2, sodium modification: dissolving 20g sodium phosphate in 100ml water to obtain solution, gradually heating the stirring kettle to 65 deg.C, adding 100ml sodium phosphate solution, and stirring at 200 rpm/MIN for 60 MIN.
And step 3, drying: heating to 100 deg.C and stirring at 100 rpm for 5 hr until the water content is 8%.
Step 4, crushing: taking out the dried product, and placing the dried product in a mechanical crusher for crushing to obtain the fineness of 300 meshes.
Step 5, organizing and acidifying: adding 15gKH570 silane coupling agent into 70ml deionized water, stirring uniformly, adding 10g ammonium phosphate into the solution, and continuing stirring until uniform; and (3) putting the powder obtained in the step (4) into a high-speed stirring kettle, stirring at a high speed, adding the powder into a mixed solution of a silane coupling agent and an ammonium phosphate solution, stirring for 15MIN, adding 3ml of acetic acid, and continuing stirring at a high speed for 30 MIN.
Step 6, refining: taking out the uniformly stirred powder, placing the powder in a jet mill for grinding to the fineness of 2500 meshes, adding the powder into a sealed plastic bag, and sealing and storing for 7 days to obtain the organic montmorillonite prepared by the dry method.
Through the steps, the dry-method organic montmorillonite is prepared.
Example 4
The results of the interlayer spacing, temperature resistance and particle fineness measurements of the organic montmorillonite obtained in examples 1-3 are shown in Table 1 below.
Table 1 results of measuring characteristics of organic montmorillonite obtained in example
| Performance of | Unit of | Example 1 | Example 2 | Example 3 | Original soil |
| Layer spacing | nm | 1.35 | 1.41 | 1.36 | 1.0 |
| Fineness of particle | Eyes of a user | 2000 | 2000 | 2500 | 200 |
It can be seen that the interlamellar spacing of the organic montmorillonite obtained by the method is improved to a certain extent compared with that of the raw material, and the expansion of the interlamellar spacing is not obvious along with the increase of the addition amount; the particle fineness is obviously improved;
having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (4)
1. A dry method preparation method of organic montmorillonite is characterized in that: the method comprises the following steps:
step 1, emulsification: taking montmorillonite, stirring in a stirring kettle, adding polyvinyl alcohol emulsion, and stirring for 20-30min to make the materials uniform;
step 2, sodium modification: gradually heating the uniform material obtained in the step 1 to 60-80 ℃, adding a sodium phosphate solution, and stirring for 50-60 min;
and step 3, drying: continuously heating the mixture obtained in the step 2 to 100 ℃, and stirring for 3-5 hours until the product is dried;
step 4, crushing: taking out the dried product obtained in the step (3), and putting the dried product into a mechanical crusher for crushing until the preset fineness range is reached;
step 5, organizing and acidifying: adding a silane coupling agent into deionized water, stirring uniformly, adding ammonium phosphate, and continuously stirring uniformly to form a mixed solution of the silane coupling agent and the ammonium phosphate; putting the powder crushed in the step (4) into a high-speed stirring kettle, stirring at a high speed, adding the powder into the mixed solution of the silane coupling agent and the ammonium phosphate, stirring for 15min, adding acetic acid, and continuing stirring at a high speed for 30 min;
step 6, refining: taking out the product obtained in the step 5, putting the product into an airflow grinder, grinding the product to a preset fineness, adding the product into a sealed plastic bag, and sealing and storing the product for 7 days to obtain the organic montmorillonite prepared by the dry method;
in the step 1, the montmorillonite is calcium-based montmorillonite; the mass ratio of the montmorillonite to the polyvinyl alcohol is (500-: preparing 5ml of the mixture; the stirring speed is 80-150 r/min;
in the step 2, the sodium phosphate solution refers to a solution with the mass ratio of sodium phosphate to water being 1 (10-50), the mass ratio of the addition amount of the sodium phosphate solution to the montmorillonite in the step 1 is 1 (80-200), and the stirring speed is 200-400 r/min;
in the step 5, the silane coupling agent is one of KH560, KH580, KH791, KH792, KH901 and KH 902; the mass ratio of the silane coupling agent to the montmorillonite in the step 1 is 1 (100-300), and the mass ratio of the deionized water to the silane coupling agent is 5-10: 1; the mass ratio of ammonium phosphate to the montmorillonite in the step 1 is as follows: 1 (200-500); the stirring speed is 600-1200 r/min;
the mass ratio of the ammonium phosphate in the mixed liquid of the silane coupling agent and the ammonium phosphate is 8-15%.
2. The dry process for preparing organo montmorillonite as claimed in claim 1, which comprises: in the step 3, the stirring speed is 80-150 r/min, and the product drying means that the water content in the product is less than or equal to 10% by mass.
3. The dry process for preparing organo montmorillonite as claimed in claim 1, which comprises: the predetermined fineness range in the step 4 is 300-800 meshes.
4. The dry process for preparing organo montmorillonite as claimed in claim 1, which comprises: the predetermined fineness in the step 6 is 1500-3000 meshes.
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