CN106221292A - A kind of wear-resisting span carrys out polyimide modified pearl filler - Google Patents
A kind of wear-resisting span carrys out polyimide modified pearl filler Download PDFInfo
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- CN106221292A CN106221292A CN201610546926.XA CN201610546926A CN106221292A CN 106221292 A CN106221292 A CN 106221292A CN 201610546926 A CN201610546926 A CN 201610546926A CN 106221292 A CN106221292 A CN 106221292A
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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
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/021—Calcium carbonates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/12—Unsaturated polyimide precursors
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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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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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
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
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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
- C01P2006/21—Attrition-index or crushing strength of granulates
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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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- Health & Medical Sciences (AREA)
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Abstract
nullA kind of wear-resisting span carrys out polyimide modified pearl filler，It is prepared from the following raw materials in parts by weight: Paris white 200 parts、Enuatrol 30 50 parts、Dodecylbenzene sodium sulfonate 0.5 2 parts、Sodium bicarbonate 13 parts、Styrene 48 parts、Potassium peroxydisulfate 0.2 0.5 parts、Aerosil 35 parts、Organobentonite 23 parts、Absolute methanol 30 40 parts、Aluminate coupling agent 0.5 2 parts、Carborundum 35 parts、Graphene 12 parts、Hydrogen peroxide 80 100 parts、Peroxidase 8 10 parts、Triton X-100 68 parts、Dimethylformamide 200 250 parts、5 hydroxylevulinic acids 12 parts、4，4 diphenyl methane BMIs 23 parts、Diethyl malonate 23 parts、Catalyst 0.5 1 parts、23 parts of dimethyl dimercapto 2-ethyl hexyl ethanoate stannum、Hydroxy silicon oil 23 parts、Acetone in proper、Deionized water is appropriate.
Description
Technical field
The present invention relates to a kind of pearl filler, be specifically related to a kind of wear-resisting span and carry out polyimide modified calcium carbonate
Filler.
Background technology
Calcium carbonate is the functional inorganic filling that a class is important, has cheap, rich reserves, stable performance, Yi Jia
Work, the advantage such as nontoxic, it is possible to significantly improve drawing abillity, physical property and reduce production cost etc., extensively
It is applied to the fields such as plastics, rubber, coating, papermaking.Owing to there is the hydroxyl that hydrophilic is stronger on its surface of calcium carbonate, present stronger
Alkalescence, the calcium carbonate that this hydrophilic thin oil properties makes is poor with the affinity of organic polymer, is easily formed aggregation, causes at height
In polymers, part is disperseed uneven, thus causes boundary defect between bi-material, and directly application effect is bad, and calcium carbonate is made
For filler, the performance such as its acid resistance, smoothness, whiteness need to improve further, therefore, makees to improve the reinforcement of calcium carbonate
With and dispersive property in the composite and the physical property of modified calcium carbonate filled composite materials, it is necessary to use difference
Surface modifier and processing method calcium carbonate powder is carried out surface modification, and then widen the application of calcium carbonate.
Polymer/inorganic particle composite is a kind of new material, which overcomes simple inorganic particulate and is difficult to processing, has
The shortcomings such as machine macromolecule intensity is relatively low, less stable, under cooperative effect, it is possible to obtain than inorganic particulate and organic polymer
Update, more excellent performance, improve the performance such as the stability of joint product and dispersibility in organic facies, mechanical strength, this
Invention utilization carrys out polyimides calcium carbonate surface glycerol polymerization span and is modified calcium carbonate processing, and even at Aluminate
Carborundum, Graphene and calcium carbonate tight bond under the effect of connection agent, solve the hydrophilic oleophobic of carbonic acid carbon, poor dispersion, easily
Settle, mechanical strength is the highest and polymer compatibility difference is unable to reach the problems such as potentiation, improves the application model of calcium carbonate
Enclose.
Summary of the invention
It is an object of the invention to, it is provided that a kind of wear-resisting span carrys out polyimide modified pearl filler, for reality
Existing above-mentioned purpose, the technical solution used in the present invention is as follows:
A kind of wear-resisting span carrys out polyimide modified pearl filler, it is characterised in that described calcium carbonate is by following heavy
The raw material of amount part is made: Paris white 200 parts, enuatrol 30-50 part, dodecylbenzene sodium sulfonate 0.5-2 part, sodium bicarbonate 1-
3 parts, styrene 4-8 part, potassium peroxydisulfate 0.2-0.5 part, aerosil 3-5 part, organobentonite 2-3 part, absolute methanol
30-40 part, aluminate coupling agent 0.5-2 part, carborundum 3-5 part, Graphene 1-2 part, hydrogen peroxide 80-100 part, peroxidase
8-10 part, Triton X-100 6-8 part, dimethylformamide 200-250 part, 5-hydroxylevulinic acid 1-2 part, 4,4-
Diphenyl methane BMI 2-3 part, diethyl malonate 2-3 part, catalyst 0.5-1 part, dimethyl dimercapto acetic acid
Different monooctyl ester stannum 2-3 part, hydroxy silicon oil 2-3 part, acetone in proper, deionized water are appropriate.
Described wear-resisting span carrys out polyimide modified pearl filler, it is characterised in that described calcium carbonate by
Following steps prepare:
(1) enuatrol adding deionized water dissolving and makes the aqueous solution sodium oleate of 1%, electric stirring 5-10min also rises high-temperature extremely
50-60 DEG C, add calcium carbonate stirring 1.5-2h, stand sucking filtration after 4-6h after having stirred, be washed with deionized, 70-80 DEG C
Dry；Calcium carbonate after drying is added in the four-necked bottle with driven stirring rod and reflux condensing tube, adds appropriate water and stirs
Mix and be allowed to into serosity, stop stirring and add dodecylbenzene sodium sulfonate and sodium bicarbonate, in a nitrogen atmosphere after stirring 0.5-1h
Add styrene, after mixture is warming up to 70-80 DEG C, drip persulfate aqueous solution, react 8-10h, centrifugal, deionized water
Washing, it is standby that 70-80 DEG C of drying dry, pulverize 150-200 mesh sieve；
(2) by adding after organobentonite and aerosil mix homogeneously, absolute methanol activates 0.5-1h, then grind 2-
3h less than 5 μm to particle diameter, adds deionized water ultrasonic disperse uniform, transfers to add in flask the product of step (1) gained
Thing, liter high-temperature is to 80-100 DEG C, and the ultrasonic methanol that is back to volatilizees, and dries；
(3) utilize hydrogen peroxide and peroxidase that the product of step (2) gained is carried out pretreatment, introduce activity hydroxyl on its surface
Base, obtains activity hydroxy product.
(4) by activity hydroxy product ultrasonic disperse in dimethylformamide, add 5-hydroxylevulinic acid, 4,4-bis-
Phenylmethane BMI, diethyl malonate, catalyst, 70-80 DEG C of stirring reaction 8-10h, obtain span and carry out polyamides
Imines prepolymer-calcium carbonate；
(5) span that other residual components addition step (4) obtains is come in polyimide preformed polymer-calcium carbonate, ultrasonic 2-3h,
Filter, use deionized water, washing with acetone 2-3 time respectively, 50-60 DEG C of drying, grind 20-30min, cross 150-200 mesh sieve, obtain
A kind of wear-resisting span carrys out polyimide modified pearl filler.
Described catalyst is the metallocene complex of (i) (IV) race metal, and described metallocene comprises at least two ring penta
Diene fundamental mode part.
The invention have the benefit that utilization carrys out polyimides calcium carbonate surface glycerol polymerization span and carries out calcium carbonate
Modification so that the performance of calcium carbonate changes, the performance indications such as the oil factor of powder body, viscosity, activation rate all become
Change, be more conducive to it and disperse in high molecular polymer and compatible, thus reach good filler reinforcement effect, in Aluminate coupling
Carborundum, Graphene and calcium carbonate tight bond under the effect of agent, also add pliability and the wearability of powder body, great application
It is worth.
Specific embodiment
The wear-resisting span of the present embodiment carrys out polyimide modified pearl filler, by the raw material system of following weight portion
Become: Paris white 200 parts, enuatrol 40 parts, dodecylbenzene sodium sulfonate 2 parts, sodium bicarbonate 3 parts, styrene 4 parts, persulfuric acid
0.5 part of potassium, aerosil 3 parts, organobentonite 3 parts, absolute methanol 40 parts, aluminate coupling agent 0.5 part, carborundum 3
Part, Graphene 2 parts, hydrogen peroxide 100 parts, peroxidase 10 parts, Triton X-100 8 parts, dimethylformamide 250
Part, 5-hydroxylevulinic acid 2 parts, 4,4-diphenyl methane BMI 3 parts, diethyl malonate 3 parts, catalyst 0.5
Part, 3 parts of dimethyl dimercapto 2-ethyl hexyl ethanoate stannum, hydroxy silicon oil 3 parts, acetone in proper, deionized water are appropriate.
A kind of wear-resisting span carrys out polyimide modified pearl filler, it is characterised in that described calcium carbonate is by such as
Lower step prepares:
(1) enuatrol adding deionized water dissolving and makes the aqueous solution sodium oleate of 1%, electric stirring 10min also rises high-temperature to 60
DEG C, add calcium carbonate stirring 1.5h, stand sucking filtration after 5h after having stirred, be washed with deionized, 80 DEG C of drying；After drying
Calcium carbonate be added in the four-necked bottle with driven stirring rod and reflux condensing tube, add the stirring of appropriate water and be allowed to into serosity,
Stop stirring and add dodecylbenzene sodium sulfonate and sodium bicarbonate, add styrene after stirring 0.5h in a nitrogen atmosphere, will be mixed
Compound drips persulfate aqueous solution after being warming up to 80 DEG C, reacts 8h, and centrifugal, deionized water wash, 80 DEG C of drying dry, pulverize
Cross 200 mesh sieves standby；
(2) by adding after organobentonite and aerosil mix homogeneously, absolute methanol activates 0.5h, then grind 2h extremely
Particle diameter is less than 5 μm, adds deionized water ultrasonic disperse uniform, transfers to add in flask the product of step (1) gained, rises
High-temperature is to 100 DEG C, and the ultrasonic methanol that is back to volatilizees, and dries；
(3) by peroxidase, hydrogen peroxide, Triton X-100 and the product mix homogeneously of step (2) gained, 35 DEG C
Constant temperature stirring 40min, introduces activity hydroxy, obtains the activity hydroxy compound of alienation on its surface；
(4) by activity hydroxy product ultrasonic disperse in dimethylformamide, add 5-hydroxylevulinic acid, 4,4-diphenyl
Methane BMI, diethyl malonate, catalyst, 80 DEG C stirring reaction 8h, obtain span come polyimide preformed polymer-
Calcium carbonate；
(5) span that other residual components addition step (4) obtains is come in polyimide preformed polymer-calcium carbonate, ultrasonic 3h, mistake
Filter, uses deionized water, washing with acetone 3 times respectively, and 30min is ground in 60 DEG C of drying, crosses 200 mesh sieves, obtains a kind of wear-resisting span
Carry out polyimide modified pearl filler.
The modified calcium carbonate and the unmodified calcium carbonate performance that produce the present invention compare, and obtain modified calcium carbonate ratio
Unmodified calcium carbonate oil factor reduces 56.3%, and settling volume reduces 65.8%, and viscosity reduces 62.8%, bulk density
Reduce 16.8%, modified calcium carbonate oleophilic drainage is described, good with polymer compatibility, and bulk density diminishes, explanation
Calcium carbonate dispersive property is good, is difficult to reunite.
Claims (3)
1. a wear-resisting span carrys out polyimide modified pearl filler, it is characterised in that described calcium carbonate is by following
The raw material of weight portion is made: Paris white 200 parts, enuatrol 30-50 part, dodecylbenzene sodium sulfonate 0.5-2 part, sodium bicarbonate
1-3 part, styrene 4-8 part, potassium peroxydisulfate 0.2-0.5 part, aerosil 3-5 part, organobentonite 2-3 part, without water beetle
Alcohol 30-40 part, aluminate coupling agent 0.5-2 part, carborundum 3-5 part, Graphene 1-2 part, hydrogen peroxide 80-100 part, peroxide
Enzyme 8-10 part, Triton X-100 6-8 part, dimethylformamide 200-250 part, 5-hydroxylevulinic acid 1-2 part, 4,
4-diphenyl methane BMI 2-3 part, diethyl malonate 2-3 part, catalyst 0.5-1 part, dimethyl dimercapto second
The different monooctyl ester stannum 2-3 part of acid, hydroxy silicon oil 2-3 part, acetone in proper, deionized water are appropriate.
2. carry out polyimide modified pearl filler according to the wear-resisting span described in claim 1, it is characterised in that institute
The calcium carbonate stated is prepared by following steps:
(1) enuatrol adding deionized water dissolving and makes the aqueous solution sodium oleate of 1%, electric stirring 5-10min also rises high-temperature extremely
50-60 DEG C, add calcium carbonate stirring 1.5-2h, stand sucking filtration after 4-6h after having stirred, be washed with deionized, 70-80 DEG C
Dry；Calcium carbonate after drying is added in the four-necked bottle with driven stirring rod and reflux condensing tube, adds appropriate water and stirs
Mix and be allowed to into serosity, stop stirring and add dodecylbenzene sodium sulfonate and sodium bicarbonate, in a nitrogen atmosphere after stirring 0.5-1h
Add styrene, after mixture is warming up to 70-80 DEG C, drip persulfate aqueous solution, react 8-10h, centrifugal, deionized water
Washing, it is standby that 70-80 DEG C of drying dry, pulverize 150-200 mesh sieve；
(2) by adding after organobentonite and aerosil mix homogeneously, absolute methanol activates 0.5-1h, then grind 2-
3h less than 5 μm to particle diameter, adds deionized water ultrasonic disperse uniform, transfers to add in flask the product of step (1) gained
Thing, liter high-temperature is to 80-100 DEG C, and the ultrasonic methanol that is back to volatilizees, and dries；
(3) utilize hydrogen peroxide and peroxidase that the product of step (2) gained is carried out pretreatment, introduce activity hydroxyl on its surface
Base, obtains activity hydroxy product.
(4) by activity hydroxy product ultrasonic disperse in dimethylformamide, add 5-hydroxylevulinic acid, 4,4-diphenyl
Methane BMI, diethyl malonate, catalyst, 70-80 DEG C of stirring reaction 8-10h, obtain span and carry out polyimides
Prepolymer-calcium carbonate；
(5) span that other residual components addition step (4) obtains is come in polyimide preformed polymer-calcium carbonate, ultrasonic 2-3h,
Filter, use deionized water, washing with acetone 2-3 time respectively, 50-60 DEG C of drying, grind 20-30min, cross 150-200 mesh sieve, obtain
A kind of wear-resisting span carrys out polyimide modified pearl filler.
3. the preparation method of polyimide modified pearl filler is carried out according to the wear-resisting span described in claim 2, its
Being characterised by, described catalyst is the metallocene complex of (i) (IV) race metal, and described metallocene comprises at least two ring penta
Diene fundamental mode part.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610546926.XA CN106221292A (en) | 2016-07-13 | 2016-07-13 | A kind of wear-resisting span carrys out polyimide modified pearl filler |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610546926.XA CN106221292A (en) | 2016-07-13 | 2016-07-13 | A kind of wear-resisting span carrys out polyimide modified pearl filler |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111440461A (en) * | 2020-04-30 | 2020-07-24 | 广西夏阳环保科技有限公司 | Preparation method of calcium carbonate special for plastics and coatings |
| CN111500089A (en) * | 2020-04-20 | 2020-08-07 | 池州市贵兴非矿新材料有限公司 | Active calcium carbonate and preparation method thereof |
| CN113943497A (en) * | 2020-07-17 | 2022-01-18 | 湖南磊鑫新材料科技有限公司 | Modified calcium carbonate and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105153750A (en) * | 2015-07-02 | 2015-12-16 | 青阳县恒祥炉料有限公司 | Wear-resistant surface modified calcium carbonate filler and preparation method thereof |
-
2016
- 2016-07-13 CN CN201610546926.XA patent/CN106221292A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105153750A (en) * | 2015-07-02 | 2015-12-16 | 青阳县恒祥炉料有限公司 | Wear-resistant surface modified calcium carbonate filler and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 郑永军等: "复合偶联表面处理CaCO3的新工艺研究", 《辽宁化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111500089A (en) * | 2020-04-20 | 2020-08-07 | 池州市贵兴非矿新材料有限公司 | Active calcium carbonate and preparation method thereof |
| CN111440461A (en) * | 2020-04-30 | 2020-07-24 | 广西夏阳环保科技有限公司 | Preparation method of calcium carbonate special for plastics and coatings |
| CN113943497A (en) * | 2020-07-17 | 2022-01-18 | 湖南磊鑫新材料科技有限公司 | Modified calcium carbonate and preparation method thereof |
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