CN109456621A - Organic modified sheet silicate and preparation method thereof - Google Patents
Organic modified sheet silicate and preparation method thereof Download PDFInfo
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- CN109456621A CN109456621A CN201710793627.0A CN201710793627A CN109456621A CN 109456621 A CN109456621 A CN 109456621A CN 201710793627 A CN201710793627 A CN 201710793627A CN 109456621 A CN109456621 A CN 109456621A
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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
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/309—Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
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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
- C09C1/405—Compounds of aluminium containing combined silica, e.g. mica
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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
- 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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- 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
- C09C3/06—Treatment with inorganic compounds
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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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J179/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09J161/00 - C09J177/00
- C09J179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C09J179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/08—Intercalated structures, i.e. with atoms or molecules intercalated in their structure
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- 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
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- 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
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- 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
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- 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
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- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The present invention relates to a kind of preparation methods of organosilicate.Silicate is pre-processed using the comprehensive means of thermal activation, acid processing, lithium nitrate intercalation modifying first, obtains lithium base silicate, then, modified organic intercalation agent and lithium base montmorillonite in a solvent 80 ~ 180 oCLower carry out intercalation purifies organic silicic acid saline solution, then to obtain organic modified silicate.The organic intercalation agent is R (CH2)12~18N(CH3)3Organic compound shown in R general structure, the R in general formula are chlorine atom or bromine atom.Layered silicate is muscovite subtribe and biotite subtribe.Including paragonite, muscovite, glauconite, phlogopite, biotite, zinnwaldite, lepidolite.The method of the present invention not only realizes effectively swelling for silicate layer spacing during the preparation process, and active function groups are introduced into laminated silicate interlayer, obtained organic modified sheet silicate is fluffy, easy crushing, suitable for fire resistant polyimide adhesive/laminated nm-silicate composite material, have broad application prospects.
Description
Technical field
The present invention relates to silicate modified technical fields, specifically provide a kind of organic modified sheet silicate and its preparation side
Method.
Background technique
Organic modified sheet silicate refers to be allowed to occur with phyllosilicate using organic reagent processing phyllosilicate
Physical absorption or chemical bonding form the substance with Characteristics of Organic.Due to most organic modified sheet silicates be through from
Sub- exchange process is made, so being used to form organically-modified phyllosilicate majority with certain ion-exchange capacity, such as
Montmorillonite, saponite, vermiculite, mica etc..Organic modified sheet silicate is received in polyimides adhesive/phyllosilicate in recent years
Nano composite material field has been widely used.The property of organic modified sheet silicate has the formation of nanocomposite
There is conclusive influence.Organic modified sheet silicate must have certain interlamellar spacing, so that have can for monomer or polymer chain
It can enter interlayer.
Mica silicate is the layer silicate mineral of 2:1 type, has excellent chemical property and unique physical property,
High temperature insulation, acid-fast alkali-proof, chemical property are stable, dispersion suspension is good, are widely used to apply currently as important filler
The industrial circles such as material, rubber, plastics, ceramics.But when preparing polymer/silicate composite material, due to mica silicate
Interlayer residue negative electrical charge is 1, interlayer K+It cannot be exchanged by other cations, stable structure, interlamellar spacing is difficult to expand, it is difficult to carry out
Organic intercalation.So people expect have a kind of good method of modifying to have it more to increase the distance between silicate lamella
Add broad application prospect, fire resistant polyimide adhesive/laminated nm-silicate composite material can be preferably applied for
In.
Summary of the invention
For the prior art to deficiency existing for silicate modified technology, the purpose of the present invention is intended to provide a kind of novel activity
Organosilicate and preparation method thereof, to enrich the type of active organosilicon hydrochlorate, the silicate layer for overcoming the prior art modified
The deficiencies of spacing is difficult to scale up, and the application for preparing composite material with polyimides adhesive is restricted meets plastic processing, changes
Cope with silicate requirement in the fields such as the preparation of work building materials, the preparation of nano material, biologic applications material and cosmetics.
The object of the invention is also to provide the organic modified sheet silicates of the method preparation.
A kind of preparation method of organic modified sheet silicate of the present invention includes the following steps:
1) the silicate sample after drying is calcined in resistance furnace；
2) appropriate calcining sample is taken, is stirred to react to obtain acidification silicate in nitric acid solution；
3) appropriate acidified sample is taken, obtains lithium base silicate with appropriate lithium nitrate hybrid reaction；
4) lithium base phyllosilicate is added in water, forms stable suspension；
5) organic intercalation agent of acidification is added in the suspension of phyllosilicate, mixed method is magnetic agitation with shape
At organic silicic acid saline solution.Purifying gained organic silicic acid saline solution, to obtain organosilicate.
The calcination temperature is 400 ~ 800 oC, 0.5 ~ 2h of calcination time, nitric acid solution concentration is 2 ~ 5mol/L.
The dosage of the lithium nitrate is 10 ~ 24 parts of weight, and reaction temperature is 200 ~ 400 oC, the reaction time be 8 ~ for 24 hours.
The suspension of the mixed silicate and the organic intercalation agent aqueous solution of acidification, be magnetic agitation, whipping temp 80 ~
180 oC, the reaction time be 5 ~ for 24 hours.
The organic intercalation agent is alkyl trimethyl ammonium bromide class, and alkyl chain length is 12 carbon to 18 carbon.It is described
Intercalator can be quaternary ammonium salts agent, can be alkyl trimethyl ammonium bromide class, and alkyl chain length is 12 to 18 carbon.Example
Such as dodecyl trimethyl ammonium bromide, cetyl trimethylammonium bromide or Cetyltrimethylammonium bromide.
For silicate of the invention after appropriate organic process, the entrance of organic cation can increase the interlamellar spacing of silicate,
Improve the interstratified structure and surface property of silicate, making organosilicate in a suitable organic solvent has good dispersibility,
By a kind of organic modified sheet silicate of the present invention, with suitable polymerization system by after certain process combining
Obtain nano composite polymer/laminated silicate material.
Organic modified sheet silicate prepared by the present invention, which is mainly used in, prepares fire resistant polyimide adhesive/stratiform
Silicate nano level composite material, has broad application prospects.
Compared with prior art, the present invention the advantages and benefits of the present invention are:
1, organic modified sheet silicate interlamellar spacing prepared by the present invention is greater than the layer of common quaternary ammonium salt-modified phyllosilicate
Spacing, it is general up to 8 nanometers or more, expand the application range of silicate.
2, organosilicate prepared by the present invention is set by common material with processing without complicated reaction process
It is standby, intercalator can be introduced into the interlayer of phyllosilicate, by this organic modified sheet silicate and suitable condensate
After being compound, the high-efficient nanocomposite of intercalation can be made.
3, organic modified sheet silicate prepared by the present invention, which is mainly used in, prepares fire resistant polyimide
Adhesive/laminated nm-silicate composite material, has broad application prospects.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, fields and skilled person, according to foregoing invention content to this hair
The modifications and adaptations that bright specific embodiment makes non-intrinsically safe are not difficulty, and such equivalent forms equally fall within the application institute
Attached claims limited range.
In the following embodiments unless otherwise indicated, related component percentages are weight percentage, related
Component number is parts by weight.
Embodiment 1
By the silicate sample after drying 500 in resistance furnace oCCalcine 0.5h；Appropriate calcining sample is taken, in 3mol/L nitric acid
It is stirred to react 2h in solution and obtains acidification silicate；Appropriate acidified sample is taken, mixes 200 with the lithium nitrate of 12 parts of qualityoC reaction
8h obtains lithium base silicate；Lithium base phyllosilicate is added in water, forms stable suspension；By the organic intercalation agent of acidification
It is added in the suspension of lithium base phyllosilicate, 120o8h is reacted under C.Purifying gained organic silicic acid saline solution, with
To organic modified silicate.X-ray diffraction (XRD) test result of the organically-modified sericite of gained shows its interlamellar spacing by original
1.98 nanometers of sample increase to 5.3 nanometers.
Embodiment 2
By the silicate sample after drying 500 in resistance furnace oCCalcine 0.5h；Appropriate calcining sample is taken, in 3mol/L nitric acid
It is stirred to react 2h in solution and obtains acidification silicate；Appropriate acidified sample is taken, mixes 200 with the lithium nitrate of 12 parts of qualityoC reaction
8h obtains lithium base silicate；Lithium base phyllosilicate is added in water, forms stable suspension；By the organic intercalation agent of acidification
It is added in the suspension of lithium base phyllosilicate, 150o8h is reacted under C.Purifying gained organic silicic acid saline solution, with
To organic modified silicate.X-ray diffraction (XRD) test result of the organically-modified sericite of gained shows its interlamellar spacing by original
1.98 nanometers of sample increase to 5.52 nanometers.
Embodiment 3
By the silicate sample after drying 500 in resistance furnace oCCalcine 0.5h；Appropriate calcining sample is taken, in 3mol/L nitric acid
It is stirred to react 2h in solution and obtains acidification silicate；Appropriate acidified sample is taken, mixes 200 with the lithium nitrate of 12 parts of qualityoC reaction
8h obtains lithium base silicate；Lithium base phyllosilicate is added in water, forms stable suspension；By the organic intercalation agent of acidification
It is added in the suspension of lithium base phyllosilicate, 120o8h is reacted under C.Purifying gained organic silicic acid saline solution, with
To organic modified silicate.X-ray diffraction (XRD) test result of the organically-modified sericite of gained shows its interlamellar spacing by original
1.98 nanometers of sample increase to 5.54 nanometers.
Embodiment 4
Organic sericite is added in N- methyl arsenic pyrrolidone solvent, stable suspension is obtained；By diamine monomer 4,4'- bis-
Diaminodiphenylmethane and 2, bis- [4- (4- amino-benzene oxygen) phenyl] propane of 2-, is added in N- methyl arsenic pyrrolidone solvent,
Nitrogen atmosphere protects lower stirring and dissolving, and dried 3,3' are then added portionwise, 4,4'- benzophenone tetracid dianhydride monomers, room temperature
Under be stirred to react, obtain flaxen thick polyamic acid solution, wherein adding 4,4'- diaminodiphenylmethane and 2,2- is bis-
The ratio between the amount of substance of [4- (4- amino-benzene oxygen) phenyl] propane 1:1.5, the amount of substance of 3,3', 4,4'- benzophenone tetracid dianhydrides
With the sum of the amount of substance of bis- [4- (4- amino-benzene oxygen) phenyl] propane of two kinds of diamines 4,4'- diaminodiphenylmethane and 2,2- it
Than for 1:1, the content of polyimides is 15%(mass in solution), organic sericite and polyimides mass ratio are 7:93；Will
The polyamic acid solution casting film-forming arrived, divides gradient to carry out hot imidization reaction, and concrete technology is successively 90oC keeps the temperature 1 h,
Again 140oC keeps the temperature 0.5 h, 240oC keeps the temperature 0.5 h, 300oC keeps the temperature 1 h.
The sericite modified polyimides adhesive material of preparation has following performance: T5It is 515oC, glass transition temperature
Degree 380oC.Room temperature and 250oC, 300oC, 350oThe adhesion strength of C is respectively 21.52,5.75,4.18,2.85 MPa.This condition
Under, pure polyimides adhesive has following performance: T5 478oC, glass transition temperature 302oC.Room temperature and 250oC,
300oC, 350oThe adhesion strength of C is respectively 15.65,4.21,2.51,1.97 MPa.
Claims (7)
1. the production technology of organosilicate, it is characterised in that the following steps are included:
1) the silicate sample after drying is calcined in resistance furnace；
2) appropriate calcining sample is taken, is stirred to react to obtain acidification silicate in nitric acid solution；
3) appropriate acidified sample is taken, obtains lithium base silicate with appropriate lithium nitrate hybrid reaction；
4) lithium base phyllosilicate is added in water, forms stable suspension；
5) organic intercalation agent of acidification is added in the suspension of lithium base phyllosilicate, mixed method is stirred for magnetic force
It mixes to form organic aqueous silicate solution, purifying gained organic silicic acid saline solution, to obtain organosilicate.
2. the preparation method of organosilicate as described in claim 1, it is characterised in that: the calcination temperature is 400 ~ 800oC, 0.5 ~ 2h of calcination time.
3. the preparation method of organosilicate as described in claim 1, it is characterised in that: the nitric acid solution concentration be 2 ~
5mol/L。
4. the preparation method of organosilicate as claimed in claim 2, it is characterised in that: the lithium nitrate/silicate
About 1000 ~ 2400w/w%, reaction temperature are 200 ~ 400oC, the reaction time be 8 ~ for 24 hours.
5. the preparation method of organosilicate as claimed in claim 2, it is characterised in that: the intercalator/silicate
About 500 ~ 2000w/w%.
6. the preparation method of organosilicate as claimed in claim 3, it is characterised in that: the silicalite suspension and acidification
Organic intercalation agent mixing temperature be 80 ~ 180 oC, the reaction time be 5 ~ for 24 hours.
7. the preparation method of organosilicate as described in claim 1, it is characterised in that: the intercalator is alkyl front three
Base ammonium bromide class, alkyl chain length are 12 carbon to 18 carbon.
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| CN201710793627.0A CN109456621A (en) | 2017-09-06 | 2017-09-06 | Organic modified sheet silicate and preparation method thereof |
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| CN201710793627.0A CN109456621A (en) | 2017-09-06 | 2017-09-06 | Organic modified sheet silicate and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110627078A (en) * | 2019-10-30 | 2019-12-31 | 武汉工程大学 | Method for preparing negative electrode material by modifying biotite through lithium ion exchange method |
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|---|---|---|---|---|
| CN1508194A (en) * | 2002-12-17 | 2004-06-30 | ϣ���ٹɷݹ�˾ | Laminar silicate intercalation compound with increased expanding volume, its preparing method and use |
| CN1544538A (en) * | 2003-11-14 | 2004-11-10 | 华南理工大学 | Organic modified phyllosilicate and method for preparing same |
| CN102816460A (en) * | 2011-06-08 | 2012-12-12 | 广达电脑股份有限公司 | Preparation method for organic montmorillonite |
| CN105505288A (en) * | 2015-12-04 | 2016-04-20 | 中南大学 | Polyimide tackiness agent and preparation method thereof |
-
2017
- 2017-09-06 CN CN201710793627.0A patent/CN109456621A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1508194A (en) * | 2002-12-17 | 2004-06-30 | ϣ���ٹɷݹ�˾ | Laminar silicate intercalation compound with increased expanding volume, its preparing method and use |
| CN1544538A (en) * | 2003-11-14 | 2004-11-10 | 华南理工大学 | Organic modified phyllosilicate and method for preparing same |
| CN102816460A (en) * | 2011-06-08 | 2012-12-12 | 广达电脑股份有限公司 | Preparation method for organic montmorillonite |
| CN105505288A (en) * | 2015-12-04 | 2016-04-20 | 中南大学 | Polyimide tackiness agent and preparation method thereof |
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| CN110627078A (en) * | 2019-10-30 | 2019-12-31 | 武汉工程大学 | Method for preparing negative electrode material by modifying biotite through lithium ion exchange method |
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