CN108395575A - A kind of polyolefin injection grade nano-calcium carbonate and its production method - Google Patents
A kind of polyolefin injection grade nano-calcium carbonate and its production method Download PDFInfo
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- CN108395575A CN108395575A CN201810163577.2A CN201810163577A CN108395575A CN 108395575 A CN108395575 A CN 108395575A CN 201810163577 A CN201810163577 A CN 201810163577A CN 108395575 A CN108395575 A CN 108395575A
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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
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with 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
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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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
- 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
- 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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- 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
- C09C3/12—Treatment with organosilicon 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
- 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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- 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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
Abstract
A kind of polyolefin injection grade nano-calcium carbonate and its production method, including the group of following parts by weight are grouped as：88~95 parts of nano-calcium carbonate, 3~6 parts of coupling agent, 0.2~3 part of ethylene bis stearamide, 1.5~3 parts of polymethyl methacrylate, 1.5~3 parts of methyl methacrylate/acrylic acid ester copolymer.The production technology of the polyolefin injection grade nano-calcium carbonate, nano-calcium carbonate and the modifier treatment of various different performances, different function is set to be combined, selected high-speed stirred mediates 800~1000 revs/min of rotating speed, 100~110 ± 1 DEG C of high-speed stirred mixture temperature, 35~45 ± 1 DEG C of stirring at low speed mixture temperature.This method effectively improves the mobility of polyolefin injecting products, release property, so that product surface is had very high smoothness and flatness, processing technology is easy, easily controllable.
Description
Technical field
The invention belongs to calcium carbonate modified fields, more particularly, to a kind of polyolefin injection grade nano-calcium carbonate and its production
Method.
Background technology
Modifying plastics processing industry and calcium carbonate industry combine, and the development of modifying plastics are promoted, in plastic industry
Technological innovation in play positive effect.Calcium carbonate is one of most important, most widely used inorganic salts.It is both at home and abroad most
One of abundant filler.The major advantage of pearl filler is that raw material sources are extensive, cheap, nontoxic.Currently, calcium carbonate is
It is widely used in the industries such as rubber, plastics, papermaking, coating, ink, medicine, food, cosmetics, calcium carbonate main function：It improves
Processing performance（Adjust viscosity, rheological property, mobile performance）；Improve dimensional stability；Reinforcing or half reinforcement；Improve printing
Energy；Change physical property（Such as heat resistance, wearability, anti-flammability, delustring, whiteness, glossiness）.And calcium carbonate is as inorganic powder
Body meterial additive has many good qualities：Cheap, cost performance is high；Whiteness value is high, meets the requirement of plastic processing enterprise；It is real
It is good with performance；To environment without destruction and pollution during manufacture and use.
Calcium carbonate is one of most important, the most inorganic particle additive used in plastic products industry, is white powder
End, nontoxic, tasteless, hardness is not high, relative density 2.71, and calcium oxide and carbon dioxide are decomposed at 825 DEG C~896.6 DEG C.
Application can also generate a large amount of environmental benefit to calcium carbonate powder in the plastic, and achievement in research in recent years shows in plastic products
When having calcium carbonate powder, calcium carbonate is possible to meeting and CO after landfill2And H2O reacts, and generates the Ca (HCO for being dissolved in water3)2And from
Open film.The micropore left will increase the area of plastic contacts surrounding air and microorganism, to promote the degradation of plastics.
Therefore, certain product requirements at least add 15% inorganic filler.
The filling-modified technology of calcium carbonate powder in the plastic is quickly grown, and calcium carbonate is not only cheap, moreover it is possible to play
Increment, the effect for reducing cost, and have significant modifying function for the matrix plastic filled, plastics can be significantly improved
The physical property of product.The material especially based on nano-calcium carbonate powder, can not only make by unique process for treating surface
The impact property (toughness) of filled plastics is significantly improved, and the tensile strength and bending modulus (rigidity) of material be also simultaneously simultaneously
It does not significantly reduce.
The production method of nanometer grade calcium carbonate has more a variety of at present, as Chinese patent CN103980733A discloses one kind
" high-dispersion nano grade calcium carbonate synthesis modification method ", the applying date be：2014.05.26, publication date is：2014.08.13, it is
By first preparing Ca (OH)2Thick slurries, by separator separation be aged again after, be added fatty alcohol polyoxyethylene ether after grind,
Add crystal controlling agent and modifying agent enter in multifunctional calcium carbonate reaction kettle, after obtain high-dispersion nano grade calcium carbonate at
Product.But this method and process is complex, and cost is also excessively high, and is also not suitable for plastic processing industry.It is also special just like Chinese
Sharp CN104087028A discloses a kind of preparation method of PVC advertisement films special-purpose nanometer grade calcium carbonate, and the applying date is：
2014.06.19, publication date is：2014.10.08, it is to use carbon atom number for the saponification liquor of 8-18 saturated fatty acids
The poly- naphthalene formaldehyde sulfonate salt for being 3000-6000 with molecular weight is modifying agent, and nano-calcium carbonate is carried out two layers of cladding, control respectively
It is 16-25m to make ripe slurry specific surface area2/ g obtains the Nano calcium carbonate dedicated product of PVC advertisement films.This method and process is not multiple
It is miscellaneous, but cost is higher, it is larger using limitation, it is not suitable for mass producing.It is also public just like Chinese patent CN101544390A
Opened " a method of preparing nano-calcium carbonate ".The applying date is：2009.05.07, publication date is：2009.09.30 it is logical
The preparation of freezing carbonizatin method is crossed, will be carbonized after quicklime slaking, then is dehydrated up to nanometer grade calcium carbonate.This method and process compared with
Simply, cost is also less, but impurities amount is larger in component, and product purity is inadequate, need in terms of plastics processing and applications
It improves.Also as Chinese patent CN105217672A is disclosed " a kind of preparation method of low-water-content nanometer grade calcium carbonate ".Add
Entering mass fraction is：50~100 parts of lime stone, 1~5 part of sodium hydroxide, 3~10 parts of stearic acid, 1~5 part of sugar, sugar are white sand
Sugar.It is specially measured by formula and digests impurity elimination, heating, drying is sieved up to low-water-content nanometer grade calcium carbonate.Above-mentioned nano-sized carbon
Sour calcium has the shortcomings that poor fluidity, release property are poor, dispersibility is not high in processed and applied, to limit plastic injection production
In application.
Invention content
The primary purpose of the present invention is that nano-calcium carbonate is molded the shortcoming in production application in polyolefin, and provide
A kind of good fluidity, release property in manufacture of polyolefins processed and applied be good, good dispersion injection molding special-purpose nanometer grade calcium carbonate；
Another object be to provide a kind of simple process, easily operated polyolefin injection grade nano-calcium carbonate production method.
The present invention easily reunites from nano-calcium carbonate grain size is too thin to which poor fluidity, release property difference are started with, and pointedly selects
It is used in combination with a variety of modifying agent, solves nanometer materials and reunite and improve mobility, using high-speed stirred kneading process and low
Speed stirring low temperature is quickly cooled down the production method of sizing.
Realize that the primary and foremost purpose scheme of the present invention is as follows：
A kind of polyolefin injection grade nano-calcium carbonate, includes the component of following parts by weight：88~95 parts of nano-calcium carbonate, coupling
3~6 parts of agent, 0.2~3 part of ethylene bis stearamide, 1.5~3 parts of polymethyl methacrylate, methyl methacrylate/propylene
1.5~3 parts of acid ester copolymer.
A kind of polyolefin injection grade nano-calcium carbonate as described above, nano-calcium carbonate grain size are 30~50 nanometers.
A kind of polyolefin injection grade nano-calcium carbonate as described above, coupling agent includes monoalkoxytitanates, silane.It is single
Alkoxy titanates and silane coupling agent are surface active modifiers, are used using compound proportioning, improve material interface state, carry
Polymolecularity and compatibility；Ethylene bis stearamide improves resin melting viscosity, improves mobility and release property；Polymethyl
Sour methyl esters and methyl methacrylate/acrylic acid ester copolymer improve processing performance and flexibility.
Realize that the scheme of another object of the present invention is as follows：
A kind of production method of polyolefin injection grade nano-calcium carbonate, high-speed stirred mediates 800~1000 revs/min of rotating speed, high
Fast stir mixing temperature is 100~110 ± 1 DEG C, 10-15 minutes time, 400~500 turns of rotating speed of low speed cooling stirring kneading/
Minute, stirring at low speed mixture temperature is 35~45 ± 1 DEG C, 5-8 minutes time.Make nano-calcium carbonate and various different performances, no
The modifier treatment of congenerous is compound, and nano-calcium carbonate is made to have the characteristics that high fluidity, release property, polymolecularity, selectes height
800~1000 revs/min of rotating speed is mediated in speed stirring, and nano-calcium carbonate is made to reach polyolefin injection grade requirement, processing technology
Simplicity, it is easily controllable.
The remarkable advantage of the present invention has：
2. the polyolefin injection grade nano-calcium carbonate has selected high-quality and efficient surface active modifier, in nano-calcium carbonate and gather
A boundary layer is formed between alkene, boundary layer can transmit stress, to enhance between Nano-Calcium Carbonate and polyolefin
Adhesive strength, improves the performance of polyolefin injected plastics material, while being also prevented from other media to contacting permeation, improves interface
State.Promote polyolefin plasticizing, improve thermoplastic melt rheological property, improve thermoelasticity state under melt mechanical property and
Improve the comprehensive functions such as the presentation quality of polyolefin injection-molded item.
Specific implementation mode
Below by specific embodiment, the present invention will be further described.
Embodiment 1, a kind of polyolefin injection grade nano-calcium carbonate are made of the raw material of following weight part ratio：Nano-calcium carbonate
95 parts of calcium, 1.5 parts of monoalkoxytitanates, 1 part of silane coupling agent, 1.5 parts of ethylene bis stearamide, polymethyl methacrylate
1.5 parts, 1 part of methyl methacrylate/acrylic acid ester copolymer.
Embodiment 2, a kind of polyolefin injection grade nano-calcium carbonate are made of the raw material of following weight part ratio：Nano-calcium carbonate
93 parts of calcium, 2 parts of monoalkoxytitanates, 1 part of silane coupling agent, 1 part of ethylene bis stearamide, 2 parts of polymethyl methacrylate,
2 parts of methyl methacrylate/acrylic acid ester copolymer.
Embodiment 3, a kind of polyolefin injection grade nano-calcium carbonate are made of the raw material of following weight part ratio：Nano-calcium carbonate
93 parts of calcium, 1 part of monoalkoxytitanates, 2 parts of silane coupling agent, 1.5 parts of ethylene bis stearamide, polymethyl methacrylate 3
Part, 1 part of methyl methacrylate/acrylic acid ester copolymer.
Embodiment 4, a kind of polyolefin injection grade nano-calcium carbonate are made of the raw material of following weight part ratio：Nano-calcium carbonate
91 parts of calcium, 2 parts of monoalkoxytitanates, 1.5 parts of silane coupling agent, 1 part of ethylene bis stearamide, polymethyl methacrylate 3
Part, 2.5 parts of methyl methacrylate/acrylic acid ester copolymer.
A kind of production method of polyolefin injection grade nano-calcium carbonate of the various embodiments described above is：By nano-calcium carbonate with it is various
Different performance, different function modifying agent high speed processing mediate, specific production technology：Dispensing → high-speed stirred → low speed is cold
But stirring → product storehouse → metering → packaging → qualification storage.
A kind of above-mentioned polyolefin injection grade nano-calcium carbonate preparation technology parameter is：1000 turns of rotating speed of high-speed stirred kneading/
Minute, high-speed stirred mixture temperature is 105 ± 1 DEG C, 10-15 minutes time, and rotating speed 400~500 is mediated in low speed cooling stirring
Rev/min, stirring at low speed mixture temperature is 40 ± 1 DEG C, 5-8 minutes time.
The performance detection of a kind of polyolefin injection grade nano-calcium carbonate and ordinary calcium carbonate to the present invention is compared as follows：
First, in accordance with《Molecular sieve sedimentating density measuring method》The accumulation of calcium carbonate is close before and after GB/T6286-1986 measurement processing
A kind of polyolefin injection grade nano-calcium carbonate and ordinary calcium carbonate, are then added in 15% ratio in PP resins by degree respectively,
Sample is made；It presses《Thermoplastic plastic pipe Erichsen test method》GB/T8804.2-2003 tests two kinds and sample is made
Mechanical property,；It presses《Plastics and the detection of manufactured goods glossiness》GB/T8807-1988 detects glossiness；Comparing result table is as follows：
As can be seen from the above table, a kind of loosely-packed that sample is made than ordinary calcium carbonate for polyolefin injection grade nano-calcium carbonate is close
Degree becomes smaller, and illustrates that calcium carbonate split is fully dispersed, still further it can be seen that a kind of treated polyolefin injection grade nano-calcium carbonate ratio
The mechanical property of sample is made in ordinary calcium carbonate and glossiness is all improved.
Claims (5)
1. a kind of polyolefin injection grade nano-calcium carbonate, it is characterised in that include the component of following parts by weight：Nano-calcium carbonate
88~95 parts, 3~6 parts of coupling agent, 0.2~3 part of ethylene bis stearamide, 1.5~3 parts of polymethyl methacrylate, methyl-prop
1.5~3 parts of e pioic acid methyl ester/acrylate copolymer.
2. a kind of polyolefin injection grade nano-calcium carbonate according to claim 1, it is characterised in that：Nano-calcium carbonate grain size
It is 30~50 nanometers.
3. a kind of polyolefin injection grade nano-calcium carbonate according to claim 1, it is characterised in that coupling agent includes single alkane
Oxygroup titanate esters, silane.
4. according to a kind of production method of any polyolefin injection grade nano-calcium carbonate of claims 1 to 3, feature exists
In：By nano-calcium carbonate, monoalkoxytitanates, silane coupling agent, ethylene bis stearamide, polymethyl methacrylate, first
Base methyl acrylate/acrylate copolymer high-speed kneading.
5. a kind of production method of polyolefin injection grade nano-calcium carbonate according to claim 3, it is characterised in that：At a high speed
800~1000 revs/min of rotating speed is mediated in stirring, and high-speed stirred mixture temperature is 100~110 ± 1 DEG C, and low speed cooling stirring is mediated
400~500 revs/min of rotating speed, stirring at low speed mixture temperature is 35~45 ± 1 DEG C, and nano-calcium carbonate and modifying agent high speed is made to pinch
It closes.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992561A (en) * | 2014-05-13 | 2014-08-20 | 永高股份有限公司 | Method of preparing pipe fittings from polyolefin master batch |
| CN104861338A (en) * | 2014-12-29 | 2015-08-26 | 殷培花 | High-performance low-cost polyvinyl chloride insulating cable material and preparation method thereof |
| CN106543558A (en) * | 2016-10-17 | 2017-03-29 | 江西广源新材料有限公司 | A kind of polypropylene filler parent granule and preparation method thereof |
-
2018
- 2018-02-27 CN CN201810163577.2A patent/CN108395575A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992561A (en) * | 2014-05-13 | 2014-08-20 | 永高股份有限公司 | Method of preparing pipe fittings from polyolefin master batch |
| CN104861338A (en) * | 2014-12-29 | 2015-08-26 | 殷培花 | High-performance low-cost polyvinyl chloride insulating cable material and preparation method thereof |
| CN106543558A (en) * | 2016-10-17 | 2017-03-29 | 江西广源新材料有限公司 | A kind of polypropylene filler parent granule and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 汪多仁: "《绿色纳米化学品（2007年7月第1版）》", 31 July 2007, 科学技术文献出版社 * |
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