CN108003385A - A kind of environment-friendly modified pearl filler and preparation method thereof - Google Patents
A kind of environment-friendly modified pearl filler and preparation method thereof Download PDFInfo
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- CN108003385A CN108003385A CN201711406010.5A CN201711406010A CN108003385A CN 108003385 A CN108003385 A CN 108003385A CN 201711406010 A CN201711406010 A CN 201711406010A CN 108003385 A CN108003385 A CN 108003385A
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- calcium carbonate
- coupling agent
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- pearl filler
- modified pearl
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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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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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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
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular 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
- 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
- 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
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a kind of environment-friendly modified pearl filler and preparation method thereof.Raw material includes：Calcium carbonate, isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate coupling agent, propylene glycol monostearate coupling agent, diethylene glycol dibenzoate plasticizer, maleic anhydride grafting compatilizer, ascorbic acid.Calcium carbonate powder and water are prepared by mixing into calcium carbonate slurry first, add isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate coupling agent, propylene glycol monostearate coupling agent successively again, stir 5 10min, again diethylene glycol dibenzoate plasticizer, maleic anhydride grafting compatilizer are sequentially added toward system, stir 5 10min, heat 50 60 DEG C, ascorbic acid is added after stirring 1 2h, 1 2h is stirred under the conditions of 60 70 DEG C, finally dehydration, the high temperature drying under the conditions of 110 120 DEG C, up to modified pearl filler.
Description
Technical field
The invention belongs to calcium carbonate modified preparing technical field, and in particular to modified using silane coupling agent, plasticizer etc.
A kind of pearl filler and its method.
Background technology
Cheap, hardness is low, heat endurance and chemical stability are good, easy dry, nontoxic, nothing because having for calcium carbonate
Irritation, it is tasteless the advantages that, so largely being used in plastic processing.But calcium carbonate is directly added to resin system
In, but the mechanical property of plastic material can be made to decline comprehensively, this shortcoming of calcium carbonate powder can limit the addition of calcium carbonate
Ratio, also limits the large-scale application of calcium carbonate.
If calcium carbonate is surface-treated in advance or using advanced interface modification technology, carbonic acid can be mitigated
Harmful effect of the calcium to filled plastics mechanical property, or even the pure matrix plastic of some performance ratios is also got well.Application for many years is real
Trample and show, the calcium carbonate (popular method is referred to as activated calcium carbonate) handled by surface organic modification can not only reduce plastic products
The cost of raw material, the shock resistances of plastic products can also be improved.For the calcium carbonate of plastic processing, the particle diameter of calcium carbonate
Generally 1-10 microns, this fine particle have great specific surface area and Gibbs free energy, in thermodynamics not
Stable state.When calcium carbonate is added in resin system, due to closing on interparticle polarity absorption and Van der Waals force
Effect, particle has close to each other, the total specific surface area of reduction and the trend of surface free energy, so that calcium carbonate granule is difficult from group
Aggressiveness is converted to high degree of dispersion body.Calcium carbonate for not carrying out surface organic modification processing, when being kneaded together with resin, carbon
Sour calcium is difficult to disperse, and also is difficult to dispersed open its when high temperature and high speed is mediated.In order to improve the scattered equal of calcium carbonate
Even property and stability, it is necessary to eliminate or weaken its surface polarity and reduce its surface free energy.It is preferable scattered in order to make to have
Property and stability, generally improve its performance using auxiliary agents such as coupling agent and plasticizer.
Dioctyl phthalate (Dioctyl Phthalate), abbreviation dioctyl ester (DOP), due to good electrical property, volatilization
The features such as property is low and low temperature resistant, for a long time, be widely used in it is calcium carbonate modified, however, the toxicity of this kind of material is also more and more
Cause the concern of countries in the world, scientific research finds that phthalic acid ester is a kind of environmental estrogens material, has reproduction and hair
Toxicity is educated, therefore dioctyl phthalate is applied to modified calcium carbonate powder, has environmental hazard.And diethylene glycol (DEG) dibenzoic acid
Ester is used as the plasticizer of calcium carbonate, it have plasticizing efficiency height, small toxicity, good with polymer compatibility, volatility is low, etc.
Advantage.
The content of the invention
It is an object of the present invention to provide a kind of good using the diethylene glycol dibenzoate plasticizer modification preparation feature of environmental protection
Pearl filler.The pearl filler is made of the raw material of following parts by weight：100 parts of calcium carbonate, (the dioctyl Jiao's phosphorus of isopropyl three
Sour acyloxy) 1-2 parts of titanate coupling agent, 1-2 parts of propylene glycol monostearate coupling agent, diethylene glycol dibenzoate plasticizer
2-4 parts, maleic anhydride grafting 1-2 parts of compatilizer, 1-2 parts of ascorbic acid.
The calcium carbonate is calcium bicarbonate powder more than 400 mesh.
Above-described pearl filler, its preparation method include the following steps：
(1) suitable calcium carbonate powder is taken first, is added water and is uniformly mixed, is prepared into calcium carbonate slurry；
(2) in above-mentioned calcium carbonate slurry, isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate coupling agent, third are added successively
Glycol monostearate coupling agent, and stir 5-10min；
(3) diethylene glycol dibenzoate plasticizer, maleic anhydride grafting compatilizer are sequentially added toward system again, stir 5-10min；
(4) 50-60 DEG C will be heated in above-mentioned mixing liquid, stir 1-2h；
(5) ascorbic acid is finally added, 60-70 DEG C is heated to and stirs 1-2h；
(6) mixed system is dehydrated after reaction, obtains calcium carbonate wet feed；
By wet feed under the conditions of 110-120 DEG C high temperature drying, dry postcooling is up to modified pearl filler.
Beneficial effects of the present invention are：
(1) raw material is wide, cheap with source；
(2) the calcium carbonate powder stability prepared, good dispersion.
Embodiment
Embodiment one：
(1) first take the calcium bicarbonate powder of 400 mesh of 100g to pour into the heating container with electric stirring, it is equal to add water mixing
It is even, it is prepared into calcium carbonate slurry；
(2) in above-mentioned calcium carbonate slurry, add successively three (dioctylphyrophosphoric acid acyloxy) titanate coupling agent of 1g isopropyls,
1g propylene glycol monostearate coupling agents, and stir 5min；
(3) 2g diethylene glycol dibenzoates plasticizer, 1g maleic anhydrides grafting compatilizer are sequentially added toward system again, stir 5min；
(4) 50 DEG C will be heated in above-mentioned mixing liquid, stirs 1h；
(5) 1g ascorbic acid is finally added, 60 DEG C is heated to and stirs 1h；
(6) mixed system is dehydrated after reaction, obtains calcium carbonate wet feed；
(7) pearl filler wet feed being modified to obtain the final product in 110 DEG C of high temperature dryings, dry postcooling.
Embodiment two：
(1) take the calcium bicarbonate powder of 420 mesh of 100g to pour into the heating container with electric stirring, add water and be uniformly mixed,
It is prepared into calcium carbonate slurry；
(2) in above-mentioned calcium carbonate slurry, add successively three (dioctylphyrophosphoric acid acyloxy) titanate coupling agent of 1.5g isopropyls,
1.5g propylene glycol monostearate coupling agents, and stir 8min；
(3) 3g diethylene glycol dibenzoates plasticizer, 1.5g maleic anhydrides grafting compatilizer are sequentially added toward system, stir 8min；
(4) 55 DEG C are heated in above-mentioned mixing liquid, stirs 1.5h；
(5) 1.5g ascorbic acid is added afterwards, is heated to 65 DEG C and is stirred 1.5h；
(6) mixed system is dehydrated after answering, obtains calcium carbonate wet feed；
(7) the pearl filler that wet feed is modified to obtain the final product in 115 DEG C of high temperature dryings, dry postcooling.
Embodiment three：
(1) take the calcium bicarbonate powder of 450 mesh of 100g to pour into the heating container with electric stirring, add water and be uniformly mixed,
It is prepared into calcium carbonate slurry；
(2) in above-mentioned calcium carbonate slurry, three (dioctylphyrophosphoric acid acyloxy) titanate coupling agent of 2g isopropyls, 2g are added successively
Propylene glycol monostearate coupling agent, and stir 10min；
(3) 4g diethylene glycol dibenzoates plasticizer, 2g maleic anhydrides grafting compatilizer are sequentially added toward system, stir 10min；
(4) 60 DEG C are heated in above-mentioned mixing liquid, stirs 2h；
(5) 2g ascorbic acid is added afterwards, is heated to 70 DEG C and is stirred 2h；
(6) mixed system is dehydrated after reaction, obtains calcium carbonate wet feed；
(7) pearl filler wet feed being modified to obtain the final product in 120 DEG C of high temperature dryings, dry postcooling.
The functional calcium carbonate of the preparation of embodiment 1-3 is added in resin in 20% ratio, batten is made, is tested
Its mechanical property.Mainly include impact strength, tensile strength, the measure of bending strength.Specific method is performed with reference to following standard,
The plastics charpy impact test methods of GB/T1043-93；The plastic tensile test methods of GB/T1040-92；GB/T9341—
2000 Plastics-Oetermination of flexural properties methods, the result is shown in table 1.
Table 1
| Experimental project | Impact strength/(J/m) | Tensile strength/MPa | Bending strength/MPa |
| Embodiment 1 | 26 | 24.4 | 25.3 |
| Embodiment 2 | 28 | 25.3 | 26.6 |
| Embodiment 3 | 30 | 26.6 | 28.3 |
Claims (5)
1. a kind of environment-friendly modified pearl filler, it is characterised in that it includes the following component in terms of weight fraction：Calcium carbonate
100 parts, 1-2 parts of isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate coupling agent, propylene glycol monostearate coupling agent 1-2
Part, 1-2 parts of compatilizer of 2-4 parts of diethylene glycol dibenzoate plasticizer, maleic anhydride grafting, 1-2 parts of ascorbic acid.
2. environment-friendly modified pearl filler according to claim 1, it is characterised in that it includes in terms of weight fraction
Following component：
100 parts of calcium carbonate, 1.5 parts of isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate coupling agent, propane diols monostearate
1.5 parts of ester coupling agent, 3 parts of diethylene glycol dibenzoate plasticizer, 1.5 parts of compatilizer of maleic anhydride grafting, ascorbic acid 1.5
Part.
3. the environment-friendly modified pearl filler as described in claims 1 or 2 is any, it is characterised in that the calcium carbonate
For calcium bicarbonate powder more than 400 mesh.
A kind of 4. preparation method of environment-friendly modified pearl filler as claimed in claim 1 or 2, it is characterised in that the system
Preparation Method includes the following steps：
(1) suitable calcium carbonate powder is taken first, is added water and is uniformly mixed, is prepared into calcium carbonate slurry；
(2) in above-mentioned calcium carbonate slurry, isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate coupling agent, third are added successively
Glycol monostearate coupling agent, and stir 5-10min；
(3) diethylene glycol dibenzoate plasticizer, maleic anhydride grafting compatilizer are sequentially added toward system again, stirs 5-10min；
(4) 50-60 DEG C will be heated in above-mentioned mixing liquid, stirs 1-2h；
(5) ascorbic acid is finally added, 60-70 DEG C is heated to and stirs 1-2h；
(6) mixed system is dehydrated after reaction, obtains calcium carbonate wet feed；
(7) by wet feed under the conditions of 110-120 DEG C high temperature drying, dry postcooling is up to modified pearl filler.
A kind of 5. preparation method of environment-friendly modified pearl filler as claimed in claim 3, it is characterised in that the preparation side
Method includes the following steps：
(1) suitable calcium carbonate powder is taken first, is added water and is uniformly mixed, is prepared into calcium carbonate slurry；
(2) in above-mentioned calcium carbonate slurry, isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate coupling agent, third are added successively
Glycol monostearate coupling agent, and stir 5-10min；
(3) diethylene glycol dibenzoate plasticizer, maleic anhydride grafting compatilizer are sequentially added toward system again, stirs 5-10min；
(4) 50-60 DEG C will be heated in above-mentioned mixing liquid, stirs 1-2h；
(5) ascorbic acid is finally added, 60-70 DEG C is heated to and stirs 1-2h；
(6) mixed system is dehydrated after reaction, obtains calcium carbonate wet feed；
(7) by wet feed under the conditions of 110-120 DEG C high temperature drying, dry postcooling is up to modified pearl filler.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711406010.5A CN108003385A (en) | 2017-12-22 | 2017-12-22 | A kind of environment-friendly modified pearl filler and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711406010.5A CN108003385A (en) | 2017-12-22 | 2017-12-22 | A kind of environment-friendly modified pearl filler and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101983982A (en) * | 2010-11-19 | 2011-03-09 | 大连海事大学 | Raw material composition for preparing heavy caliber polypropylene double-wall corrugated pipe |
| CN103374162A (en) * | 2012-04-18 | 2013-10-30 | 建德市嘉和新型材料有限公司 | Toughening and rigidity-improving difunctional filling master batch and preparation method thereof |
| CN104629519A (en) * | 2015-02-02 | 2015-05-20 | 芜湖市宝艺游乐科技设备有限公司 | Magnetic polyethylene powder coating containing maleic anhydride grafted activated nano calcium carbonate and preparation method of polyethylene powder coating |
-
2017
- 2017-12-22 CN CN201711406010.5A patent/CN108003385A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101983982A (en) * | 2010-11-19 | 2011-03-09 | 大连海事大学 | Raw material composition for preparing heavy caliber polypropylene double-wall corrugated pipe |
| CN103374162A (en) * | 2012-04-18 | 2013-10-30 | 建德市嘉和新型材料有限公司 | Toughening and rigidity-improving difunctional filling master batch and preparation method thereof |
| CN104629519A (en) * | 2015-02-02 | 2015-05-20 | 芜湖市宝艺游乐科技设备有限公司 | Magnetic polyethylene powder coating containing maleic anhydride grafted activated nano calcium carbonate and preparation method of polyethylene powder coating |
Non-Patent Citations (2)
| Title |
|---|
| 化学工业出版社: "《中国化工产品大全.下卷》", 31 January 2005, 化学工业出版社 * |
| 汪多仁 主编: "《精细化工品实用生产技术手册：增塑剂化学品生产和合成工艺》", 31 August 1999, 科学技术文献出版社 * |
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Application publication date: 20180508 |