CN107400384A - A kind of preparation method of modified montmorillonoid - Google Patents
A kind of preparation method of modified montmorillonoid Download PDFInfo
- Publication number
- CN107400384A CN107400384A CN201610336051.0A CN201610336051A CN107400384A CN 107400384 A CN107400384 A CN 107400384A CN 201610336051 A CN201610336051 A CN 201610336051A CN 107400384 A CN107400384 A CN 107400384A
- Authority
- CN
- China
- Prior art keywords
- modified montmorillonoid
- preparation
- montmorillonite
- dissolved
- washed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
- C08K9/04—Ingredients treated with organic substances
-
- 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
- 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
Abstract
The present invention is to provide a kind of preparation method of modified montmorillonoid, belongs to inorganic reinforcement preparation field.Its step is as follows：（1）Montmorillonite is dissolved in ultrasound is carried out in water, add dispersant stirring, and regulation system pH；Then solution is settled, upper strata suspension is decanted, centrifuged, washed, drying, obtain purifying montmorillonite；（2）Above-mentioned purifying montmorillonite is dissolved in water, adds surfactant reaction；After the completion of reaction, product is filtered, washed, is dried, sieving produces modified montmorillonoid.The present invention compared with prior art, the advantage is that：Modified montmorillonoid dispersiveness significantly improves, the increase of thermal weight loss rate, and is improved with organic polymer resin compatibility, has certain anti-flammability.
Description
Technical field
The present invention is to provide a kind of modified montmorillonoid and preparation method thereof, belongs to inorganic reinforcement preparation field.
Technical background
Montmorillonite is stored abundant, cheap and special construction and become naturally prepares polymer nanocomposites most
Common raw clay.The chemical formula of montmorillonite is (1/2 Ca, Na)0.66(Al, Mg, Fe)4［ (Si, Al)8O20(OH)4·
NH2O, in stratiform or laminated structure, it is mingled with an alumina octahedral by two silicon-oxy tetrahedrons and piles up and form, passes through that to share oxygen former
Son forms the sandwich of sandwich form, and the thickness in monolayer of each of which crystal is 1 nm or so, and surface transverse width reaches 100
nm.These design features make it show good cation exchange capacity (CEC), strong adsorptivity and surface-active.But due to substantial amounts of
Inorganic ions is dispersed between cheating engaging layer, and it is in hydrophilic and oleophobic property to make its surface, is unfavorable for disperseing in the polymer.
The content of the invention
The purpose of the present invention is to overcome above-mentioned insufficient problem, in montmorillonite using preceding trying to purify it and surface has
Machineization be modified, there is provided a kind of montmorillonite of modification, make its product good dispersion, thermal weight loss rate increase, and with organic polymer tree
Lipid phase capacitive is improved, and has certain anti-flammability, and the enhancing or cooperative flame retardant that can be widely applied to high polymer material are modified.
Realizing the object of the invention technical solution is：First montmorillonite is purified, then organ-mmt will be purified
It is modified, product is obtained, its step is as follows：
（1）Montmorillonite is dissolved in ultrasound is carried out in water, add dispersant stirring, and regulation system pH；Then solution is settled,
Upper strata suspension is decanted, centrifuges, washs, drying, obtains purifying montmorillonite；
（2）Above-mentioned purifying montmorillonite is dissolved in water, adds surfactant reaction；After the completion of reaction, product is filtered, washed
Wash, dry, sieving produces modified montmorillonoid.
Usually, in the present invention, the dispersant is any in six inclined sodium sulphate, sodium pyrophosphate or polyethylene glycol 200.
The dispersant dosage is the 1-5% of montmorillonite quality.
In the present invention, step（1）The pH value is 3-7.
In the present invention, step（1）The middle hydrochloric acid regulation system pH value using 0.5 mol/L.
In the present invention, the surfactant is odium stearate, OTAC or titanate coupling agent
NDZ-311's is any.
The surfactant is the 1-5% of purifying montmorillonite quality.
The present invention compared with prior art, the advantage is that：Modified montmorillonoid dispersiveness significantly improves, and thermal weight loss rate increases
Greatly, and with organic polymer resin compatibility improve, there is certain anti-flammability.
Brief description of the drawings
Fig. 1 is modified montmorillonoid technological process of production sketch of the embodiment of the present invention.
Embodiment
With reference to accompanying drawing 1, the preparation method of following examples modified montmorillonoid, comprise the following steps that：
（1）A certain amount of montmorillonite is weighed, is dissolved in suitable quantity of water, is ultrasonically treated 8~20 minutes, adds 1~5% inorganic filler quality
Dispersant, stirred at 60-90 DEG C 0.5~2.5 hour, and with 0.5 mol/L hydrochloric acid regulation system pH extremely
3~7, then solution is settled, upper strata suspension is decanted, is centrifuged, is washed, drying, obtains purifying montmorillonite；
（2）Above-mentioned purifying montmorillonite is dissolved in a certain amount of water, adds the surfactant of 1~5% purifying montmorillonite quality, instead
Answer 1~3 hour, after the completion of reaction, product is filtered, washed, is dried, grinds sieving（200-1000 mesh）Modified cover is produced to take off
Soil.
Embodiment 1
（1）Weigh 80 grams of montmorillonites to be dissolved in 300 ml water, be ultrasonically treated 8 minutes, 4.0 grams of sodium pyrophosphates are added, at 90 DEG C
Stir 0.5 hour, and with 0.5 mol/L hydrochloric acid regulation system pH to 6-7, then settle solution, on decantation
Layer suspension, is centrifuged, and is washed, drying, obtains purifying montmorillonite;
（2）60 grams of purifying montmorillonites are dissolved in 300 ml water, 3.0 grams of OTACs is added, reacts 3 hours
Afterwards, product filtered, washed, dried, grinding sieving（200 mesh）Produce modified montmorillonoid.
Embodiment 2
（1）Weigh 80 grams of montmorillonites to be dissolved in 300 ml water, be ultrasonically treated 20 minutes, 0.8 gram of sodium pyrophosphate is added, at 60 DEG C
Under stir 1 hour, and with 0.5 mol/L hydrochloric acid regulation system pH to 4-5, then solution is settled, on decantation
Layer suspension, is centrifuged, and is washed, drying, obtains purifying montmorillonite;
（2）60 grams of purifying montmorillonites are dissolved in 300 ml water, 0.6 gram of odium stearate is added, after reacting 2 hours, product is taken out
Filter, washing, drying, grinding sieving（400 mesh）Produce modified montmorillonoid.
Embodiment 3
（1）Weigh 80 grams of montmorillonites to be dissolved in 300 ml water, be ultrasonically treated 15 minutes, 1.6 grams of calgons are added, 80
Stirred at DEG C 2.5 hours, and with 0.5 mol/L hydrochloric acid regulation system pH to 3-4, then solution is settled, inclined
Upper strata suspension is analysed, is centrifuged, is washed, drying, obtains purifying montmorillonite;
（2）60 grams of purifying montmorillonites are dissolved in 300 ml water, 1.8 grams of OTACs is added, reacts 3 hours
Afterwards, product filtered, washed, dried, grinding sieving（1000 mesh）Produce modified montmorillonoid.
Embodiment 4
（1）Weigh 80 grams of montmorillonites to be dissolved in 300 ml water, be ultrasonically treated 15 minutes, 2.4 grams of polyethylene glycol 200s are added, 70
Stirred at DEG C 0.5 hour, and with 0.5 mol/L hydrochloric acid regulation system pH to 5-6, then solution is settled, inclined
Upper strata suspension is analysed, is centrifuged, is washed, drying, obtains purifying montmorillonite;
（2）60 grams of purifying montmorillonites are dissolved in 300 ml water, 1.2 grams of titanate coupling agent NDZ-311s is added, reacts 2 hours
Afterwards, product filtered, washed, dried, grinding sieving（600 mesh）Produce modified montmorillonoid.
Although the present invention is detailed with preferred embodiment, but it is not intended to limit the present invention.Any this area
Technical staff, without departing from the spirit and scope of the present invention, should can with various modification can be adapted with change.
Claims (9)
1. a kind of preparation method of modified montmorillonoid, it is characterised in that methods described includes following preparation process：
（1）Montmorillonite is dissolved in ultrasound is carried out in water, add dispersant stirring, and regulation system pH；Then solution is settled, inclined
Upper strata suspension is analysed, is centrifuged, is washed, drying, obtains purifying montmorillonite；
（2）Above-mentioned purifying montmorillonite is dissolved in water, adds surfactant reaction；After the completion of reaction, product is filtered, washed
Wash, dry, sieving produces modified montmorillonoid.
2. the preparation method of modified montmorillonoid as claimed in claim 1, it is characterised in that step（1）Described in dispersant be six
It is any in inclined sodium sulphate, sodium pyrophosphate or polyethylene glycol 200.
3. the preparation method of modified montmorillonoid as claimed in claim 1 or 2, it is characterised in that step（1）Described in dispersant use
Measure as the 1-5% of montmorillonite quality.
4. the preparation method of modified montmorillonoid as claimed in claim 1, it is characterised in that step（2）Described in surfactant
For any of odium stearate, OTAC or titanate coupling agent NDZ-311.
5. the preparation method of modified montmorillonoid as described in claim 1 or 4, it is characterised in that step（2）Described in surface-active
Agent dosage is the 1-5% of purifying montmorillonite quality.
6. the preparation method of modified montmorillonoid as claimed in claim 1, it is characterised in that：Step（1）Middle sonication treatment time is 8
~20 minutes；Scattered stirring is stirred 0.5~2.5 hour under the conditions of 60-90 DEG C.
7. the preparation method of modified montmorillonoid as claimed in claim 1, it is characterised in that step（1）Middle system pH adjusted to 3~
7。
8. the preparation method of modified montmorillonoid as described in claim 1 or 7, it is characterised in that step（1）It is middle to use 0.5 mol/
L hydrochloric acid regulation system pH value.
9. the preparation method of modified montmorillonoid as claimed in claim 1, it is characterised in that：Step（2）Middle addition surfactant
Afterwards, the reaction time is 1~3 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610336051.0A CN107400384A (en) | 2016-05-20 | 2016-05-20 | A kind of preparation method of modified montmorillonoid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610336051.0A CN107400384A (en) | 2016-05-20 | 2016-05-20 | A kind of preparation method of modified montmorillonoid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107400384A true CN107400384A (en) | 2017-11-28 |
Family
ID=60394454
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610336051.0A Pending CN107400384A (en) | 2016-05-20 | 2016-05-20 | A kind of preparation method of modified montmorillonoid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107400384A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109181760A (en) * | 2018-10-30 | 2019-01-11 | 安徽海德化工科技有限公司 | A kind of production method of aromatic naphtha |
| CN111995885A (en) * | 2020-07-14 | 2020-11-27 | 南京工业大学 | Method for modifying organic montmorillonite by composite modifier |
| CN114854249A (en) * | 2022-03-25 | 2022-08-05 | 广东欧文莱陶瓷有限公司 | Metal ink for rock plate |
| CN115400612A (en) * | 2022-08-31 | 2022-11-29 | 西北工业大学 | Modified polyamide separation membrane for resisting scaling and oxidation and preparation method thereof |
| CN115611290A (en) * | 2022-11-04 | 2023-01-17 | 楚能新能源股份有限公司 | Lithiated montmorillonite and preparation method thereof, composite solid electrolyte and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1406975B1 (en) * | 2001-07-17 | 2009-03-11 | Engelhard Corporation | High strength fe-cr brown pigment with excellent weathering |
| CN102115577A (en) * | 2009-12-30 | 2011-07-06 | 上海杰事杰新材料(集团)股份有限公司 | Preparation method of polyester-ether elastomer/montmorillonite composite material |
| CN103374213A (en) * | 2012-04-26 | 2013-10-30 | 苏州达同新材料有限公司 | Preparation method of polylactic acid/montmorillonite nano composite material |
| CN104017360A (en) * | 2014-06-27 | 2014-09-03 | 南京化工职业技术学院 | Organic clay synergic flame-retardant PA6 (polyamide 6) composite material and preparation method thereof |
| CN104177769A (en) * | 2014-09-05 | 2014-12-03 | 南京百美塑业有限公司 | Novel filler-modified amino molding plastic and preparation method thereof |
-
2016
- 2016-05-20 CN CN201610336051.0A patent/CN107400384A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1406975B1 (en) * | 2001-07-17 | 2009-03-11 | Engelhard Corporation | High strength fe-cr brown pigment with excellent weathering |
| CN102115577A (en) * | 2009-12-30 | 2011-07-06 | 上海杰事杰新材料(集团)股份有限公司 | Preparation method of polyester-ether elastomer/montmorillonite composite material |
| CN103374213A (en) * | 2012-04-26 | 2013-10-30 | 苏州达同新材料有限公司 | Preparation method of polylactic acid/montmorillonite nano composite material |
| CN104017360A (en) * | 2014-06-27 | 2014-09-03 | 南京化工职业技术学院 | Organic clay synergic flame-retardant PA6 (polyamide 6) composite material and preparation method thereof |
| CN104177769A (en) * | 2014-09-05 | 2014-12-03 | 南京百美塑业有限公司 | Novel filler-modified amino molding plastic and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109181760A (en) * | 2018-10-30 | 2019-01-11 | 安徽海德化工科技有限公司 | A kind of production method of aromatic naphtha |
| CN111995885A (en) * | 2020-07-14 | 2020-11-27 | 南京工业大学 | Method for modifying organic montmorillonite by composite modifier |
| CN114854249A (en) * | 2022-03-25 | 2022-08-05 | 广东欧文莱陶瓷有限公司 | Metal ink for rock plate |
| CN114854249B (en) * | 2022-03-25 | 2023-02-10 | 广东欧文莱陶瓷有限公司 | Metal ink for rock plate |
| CN115400612A (en) * | 2022-08-31 | 2022-11-29 | 西北工业大学 | Modified polyamide separation membrane for resisting scaling and oxidation and preparation method thereof |
| CN115611290A (en) * | 2022-11-04 | 2023-01-17 | 楚能新能源股份有限公司 | Lithiated montmorillonite and preparation method thereof, composite solid electrolyte and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107400384A (en) | A kind of preparation method of modified montmorillonoid | |
| CN102259881B (en) | Method for preparing high-viscosity organic bentonite by virtue of calcium-based bentonite | |
| CN103145140B (en) | Preparation method of modified organic bentonite | |
| CN104291345B (en) | Precipitated silicon dioxide with low silanol, preparation method and use thereof | |
| CN104591199A (en) | Method for modifying montmorillonoid employing mixed surfactant and prepared modified montmorillonoid | |
| CN108584966A (en) | A kind of preparation method of the high reinforcing white carbon of high dispersive | |
| US11027981B2 (en) | Process for the preparation of silicate and its use for the preparation of precipitated silica | |
| CN108314054A (en) | A method of preparing microporous calcium silicate powder | |
| CN106495175A (en) | A kind of preparation method of organic modification montmonrillonite | |
| US10364155B2 (en) | Method of removing hydrous silica from bentonite | |
| CN103804530A (en) | Preparation method of modified powdered butadiene styrene rubber | |
| Patel et al. | Synthesis of organoclays with controlled particle size and whiteness from chemically treated Indian bentonite | |
| CN104056656A (en) | Molecular sieve with photocatalystic purification function and preparation method thereof | |
| CN107555445A (en) | A kind of aluminium magnesium silicate inorganic gel and preparation method thereof | |
| CN109250725A (en) | It is a kind of to refine montmorillonite production technology using bentonite | |
| Effenberger et al. | Synthesis and characterization of some polyacrylate/montmorillonite nanocomposites by in situ emulsion polymerization using redox initiation system | |
| Macedo et al. | Organofunctionalized RUB-18 from the intercalated precursor cetyltrimethylammonium cation | |
| CN104056594A (en) | Clay mineral absorbing material applied to water treatment and preparation method thereof | |
| EP1645544B1 (en) | Paper production comprising modified layered silicate as a microparticle | |
| US20120316264A1 (en) | Method of manufacturing organic montmorillonite | |
| US20130197137A1 (en) | Process for preparing high-purity organically modified phyllosilicates | |
| Macedo et al. | Layered inorganic/organic mercaptopropyl pendant chain hybrid for chelating heavy cations | |
| RU2433954C1 (en) | Method of modifying nanosilicates | |
| CN107200334A (en) | A kind of rice husk prepares the Efficient utilization method of white carbon | |
| RU2344067C2 (en) | Production method of modified extender for polyolefin nancomposites, modified extender and polyolefin nancomposite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171128 |