CN103360680A - Calcium carbonate filler master batch for polypropylene and polyethylene and preparation process thereof - Google Patents
Calcium carbonate filler master batch for polypropylene and polyethylene and preparation process thereof Download PDFInfo
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Abstract
The invention relates to the field of high polymer processing assistants and particularly relates to a calcium carbonate filler master batch for polypropylene and polyethylene and a preparation process thereof. The calcium carbonate filler master batch is prepared from the following ingredients in parts by weight: 60-80 parts of function-modified calcium carbonate whisker, 10-20 parts of carrier resin, 0.5-3 parts of coupling agent and 1-3 parts of lubricant, and is prepared through the steps of keeping all the ingredients at the temperature of 170-210 DEG C for 10-20 min and carrying out extrusion and granulation. The calcium carbonate filler master batch has the advantages that the cost is relatively lower, inorganic particles are uniformly dispersed in a high-polymer matrix, the combination between the inorganic particles and the high-polymer matrix is better, the calcium carbonate filler master batch has bacterium resisting and inhibiting properties, and mechanical properties, such as tensile strength, notched impact strength, wear resistance and the like, are improved.
Description
Technical field
The present invention relates to high polymer processing auxiliary agent field, be specifically related to a kind of polypropylene and polyethylene pearl filler master batch and preparation technology thereof.
Background technology
Calcium carbonate is widely used a kind of mineral filler in the polymer composite.In rubber, plastics, add calcium carbonate, can improve to a certain extent intensity, thermotolerance, wear resistance, dimensional stability and the rigidity etc. of goods, and reduce the goods cost.But the hydrophilic surface property of oil of mineral filler, make itself and macromolecular material consistency poor, therefore easily form irregular aggregate in the processing, cause macromolecular material inner disperse inhomogeneous, thereby the generation subsurface defect causes the physical and mechanical properties of goods to reduce.In order to overcome the above-mentioned shortcoming of calcium carbonate powder in using, improve itself and consistency and the dispersiveness of macromolecular material, make its packing material that becomes a kind of functional strengthening and toughening, be a focus of domestic and international powder-modified and Application Areas in recent years always.Therefore, how can be under the prerequisite that guarantees the goods properties, by certain process for modifying surface, the consumption of Effective Raise mineral filler (calcium carbonate), reduce the relative consumption of macromolecular material, reduce the cost of goods, become the important symbol of weighing a Technological Capability height.At present, the treatment process of calcium carbonate has two kinds of dry method and wet methods, and wherein the treatment effect of wet processing is better, can be so that surface treatment agent be dispersed in the surface of inorganic filler particle, and it is high to have level of automation, and dust pollution is little, low power consumption and other advantages; And the dry process technological operation is simple, is the most frequently used calcium carbonate surface treatment method.By these surface treatments, make the calcium carbonate surface become lipophilicity by wetting ability, the consistency of itself and macromolecular material and the dispersiveness in macromolecular material have been improved, thereby improved the over-all properties of goods, and because calcium carbonate powder is cheap, so surface treated calcium carbonate powder can play upgrading to all types of plastic goods this effect is fallen.
At present, the calcium carbonate surface activation process adopts stearic acid, stearate and various coupling agent (such as ferrous acid vinegar, aluminic acid vinegar, boric acid vinegar, phosphoric acid vinegar etc.) mostly, these surface treatment agents are fine to surperficial lipophilicity and the dispersed effect of improving filler, but modified effect is single, and its organic chain is usually shorter, some kind is facile hydrolysis also, can not form good stable interfacial layer, material property can not get stable raising, does not satisfy the upgrading of present plastics processing industry and falls this active demand.
Summary of the invention
The objective of the invention is for solve the easy reunion that runs into when polypropylene, polyethylene and other superpolymer add pearl filler and calcium carbonate and matrix bonding force do not cause by force product performance be subjected to calcium carbonate affect the effect that larger and existing calcium carbonate surface modifying exists single, can not form the problem that well stable interfacial layer and material property can not get stable raising
In order to reach the foregoing invention purpose, the present invention by the following technical solutions:
A kind of polypropylene and polyethylene pearl filler master batch, described polypropylene and polyethylene form with the raw material of pearl filler master batch each component by following parts by weight: function modified calcium carbonate crystal whisker 60-80 part, vector resin 10-20 part, coupling agent 0.5-3 part, lubricant 1-3 part.Calcium carbonate crystal whisker is that another novel inorganic after nano-calcium carbonate is filled, nontoxic, odorlessness, the puffy that is white in color solid (microscopically is the whiskers body) has following performance and characteristics as this product of packing material of new generation: 1: the physical strength that over-all properties is high, and in use can vibration damping, anti-skidding, noise reduction is inhaled ripple; 2: good combination property, frictional coefficient is high, and wear resisting property and resistance toheat are high; 3: stable friction performance, heat fading and hot restorability are better, particularly the filling of calcium carbonate crystal whisker more will increase rub, anti-attrition organically is unified in the individual system high temperature friction and wear superior performance; 4: product life can improve 30%; Therefore adopt calcium carbonate crystal whisker as the filler of superpolymer, but because calcium carbonate possesses the typical properties of inorganics, make its surface have very high wetting ability, thereby and because the alkaline characteristics on its surface not only cause range of application less and can't carry out effectively in conjunction with greatly reducing Properties of Polymer with superpolymer.By adopting the calcium carbonate superfine powder through modification effectively to carry out combination with superpolymer, the bonding force of raising calcium carbonate and superpolymer matrix, thus avoid causing superpolymer performance to reduce the generation of too much phenomenon owing to the adding of calcium carbonate.Vector resin helps granulation as carrier, and helps calcium carbonate crystal whisker to disperse in superpolymer matrix more easily.
As preferred version, the diameter of described function modified calcium carbonate crystal whisker is 0.5-1 μ m.Diameter is crossed conference and caused superpolymer performance to reduce too much, and is only larger through too small cost.
As preferred version, the preparation method of described function modified calcium carbonate crystal whisker is:
1) calcium carbonate crystal whisker being placed weight is that calcium carbonate crystal whisker 2-5 water doubly forms suspension liquid, adding weight in suspension liquid is the sodium stearate of calcium carbonate crystal whisker 0.3-2%, at the 50-80 ℃ of lower 20-40min that stirs, warm air drying also makes the water content of calcium carbonate crystal whisker＜1;
2) placing weight at the last product of step 1) is calcium carbonate crystal whisker 1-3 normal hexane doubly, and to add weight be the silane coupling agent of calcium carbonate crystal whisker 1-4%, the organic RE of 2-8%, at the 60-85 ℃ of lower 30-60min that stirs, removes normal hexane; This step is processed with silane coupling agent can reduce system viscosity, thereby reduces energy consumption, and silane coupling agent helps the combination of organic RE and calcium carbonate crystal whisker.By organic RE calcium carbonate crystal whisker is carried out modification, not only can increase the dyeing behavior of superpolymer matrix, organic RE has bacteriostatic action simultaneously, they have anti-inflammatory, antibiotic, anticoagulation and hypoglycemic activity, this is so that when the superpolymer that adopts filler master batch of the present invention carries out non-woven cloth products, can play good antibacterial bacteriostatic effect.Has good Ou Lian effect between calcium carbonate crystal whisker after the organic RE modification and the superpolymer matrix simultaneously, so that the dispersing uniformity of calcium carbonate crystal whisker in superpolymer matrix increases, and tensile strength, notched Izod impact strength and the abrasion resistance properties of high polymer material all are improved, the water-intake rate of material and molding shrinkage reduce simultaneously.
3) with step 2) product that obtains adopts spray art to add weight for the organic acid of its 0.3-1% in whipping process, then at 70-90 ℃ of lower warm air drying 5-10h, obtains function modified calcium carbonate crystal whisker.Because the acid resistance of calcium carbonate powders is poor, the shortcoming that surface pH value is high, its use range and usage quantity have greatly been limited, therefore in order to enlarge its use range and usage quantity, therefore with organic acid it is processed, organic acid not only can reduce the acidity on calcium carbonate superfine powder surface, and organic acid has abundant functional group, after organic acid and calcium carbonate surface reaction, can stay more organic group on the calcium carbonate surface, and can not reduce the quantity of active group, thereby can increase the bonding force between calcium carbonate crystal whisker and superpolymer matrix.
As preferred version, the temperature of described step 1) is 60-70 ℃.This temperature can access better reaction efficiency.
As preferred version, described step 2) organic RE is toxilic acid monoester rare earth, rare earth nitrate, carbonated rare earth, rare earth acetate or rare earth hydrate.
As preferred version, described step 2) temperature is 75-80 ℃.This temperature can access better reaction efficiency.
As preferred version, described vector resin is polypropylene, polyethylene or polyvinyl chloride.
As preferred version, described coupling agent is titanate coupling agent or silane coupling agent.
As preferred version, described lubricant is polyethylene wax, stearic acid or ethylene bis stearic acid amide.
A kind of polypropylene and the polyethylene preparation technology of pearl filler master batch, may further comprise the steps: be that the function modified calcium carbonate crystal whisker of 60-80 part is heated to 50-80 ℃ with parts by weight, then add successively vector resin 10-20 part, coupling agent 3-6 part, lubricant 1-3 part stirs, and at the 170-210 ℃ of lower 10-20min that keeps, extruding pelletization obtains polypropylene and polyethylene pearl filler master batch.
Beneficial effect of the present invention is: 1 provides that a kind of to have a cost relatively low, high performance filler master batch 2 has improved the dispersing uniformity of the inorganic particulate in the filler in superpolymer matrix, reduce because inorganic particulate is reunited to the disadvantageous effect of overall performance, 2 have improved the bonding force of inorganic particulate and superpolymer matrix, 4 provide the antibacterial bacteriostatic performance for superpolymer, for the health of non-woven cloth products provides condition, 5 make the tensile strength of high polymer material, notched Izod impact strength and abrasion resistance properties all are improved, the water-intake rate of material and molding shrinkage reduce simultaneously, thereby 6 have increased the addition of calcium carbonate in matrix by reducing calcium carbonate crystal whisker to the negative impact of matrix, have finally reduced cost.
Embodiment
Below by specific embodiment technical scheme of the present invention is further described explanation.
Embodiment 1:
At first, prepare function modified calcium carbonate crystal whisker:
1) be that to place weight be that the water of 3 times of calcium carbonate crystal whiskers forms suspension liquid for the calcium carbonate crystal whisker of 0.5 μ m with diameter, adding weight in suspension liquid is the sodium stearate of calcium carbonate crystal whisker 2%, at 50 ℃ of lower 30min that stir, warm air drying also makes the water content of calcium carbonate crystal whisker＜1;
2) placing weight at the last product of step 1) is the normal hexane of 3 times of calcium carbonate crystal whiskers, and to add weight be the silane coupling agent of calcium carbonate crystal whisker 1%, 5% organic RE (toxilic acid monoester rare earth), at 85 ℃ of lower 30min that stir, removes normal hexane;
3) with step 2) product that obtains adopts spray art to add weight in whipping process to be its organic acid of 0.6%, then at 90 ℃ of lower warm air drying 5h, to obtain function modified calcium carbonate crystal whisker.
Then, according to following prescription polypropylene and polyethylene are prepared burden with the pearl filler master batch: function modified calcium carbonate crystal whisker 70kg, vector resin (polypropylene) 20kg, coupling agent (silane coupling agent) 0.5kg, lubricant (polyethylene wax) 2kg.
At last, be prepared in accordance with the following steps polypropylene and polyethylene pearl filler master batch: function modified calcium carbonate crystal whisker is heated to 80 ℃, then add successively vector resin, coupling agent, lubricant stirs, and at 170 ℃ of lower 14min that keep, extruding pelletization obtains polypropylene and polyethylene pearl filler master batch.
Embodiment 2:
At first, prepare function modified calcium carbonate crystal whisker:
1) be that to place weight be that the water of 5 times of calcium carbonate crystal whiskers forms suspension liquid for the calcium carbonate crystal whisker of 0.8 μ m with diameter, adding weight in suspension liquid is the sodium stearate of calcium carbonate crystal whisker 0.3%, at 60 ℃ of lower 40min that stir, warm air drying also makes the water content of calcium carbonate crystal whisker＜1;
2) placing weight at the last product of step 1) is the normal hexane of 1 times of calcium carbonate crystal whisker, and to add weight be the silane coupling agent of calcium carbonate crystal whisker 2%, 8% organic RE (rare earth nitrate), at 60 ℃ of lower 50min that stir, removes normal hexane;
3) with step 2) product that obtains adopts spray art to add weight in whipping process to be its organic acid of 1%, then at 70 ℃ of lower warm air drying 8h, to obtain function modified calcium carbonate crystal whisker.
Then, according to following prescription polypropylene and polyethylene are prepared burden with the pearl filler master batch: function modified calcium carbonate crystal whisker 80kg, vector resin (polyethylene) 10kg, coupling agent (titanate coupling agent) 1kg, lubricant (stearic acid) 3kg.
At last, be prepared in accordance with the following steps polypropylene and polyethylene pearl filler master batch: function modified calcium carbonate crystal whisker is heated to 50 ℃, then add successively vector resin, coupling agent, lubricant stirs, and at 190 ℃ of lower 20min that keep, extruding pelletization obtains polypropylene and polyethylene pearl filler master batch.
Embodiment 3:
At first, prepare function modified calcium carbonate crystal whisker:
1) be that to place weight be that the water of 2 times of calcium carbonate crystal whiskers forms suspension liquid for the calcium carbonate crystal whisker of 1 μ m with diameter, adding weight in suspension liquid is the sodium stearate of calcium carbonate crystal whisker 1%, at 80 ℃ of lower 20min that stir, warm air drying also makes the water content of calcium carbonate crystal whisker＜1;
2) placing weight at the last product of step 1) is the normal hexane of 2 times of calcium carbonate crystal whiskers, and to add weight be the silane coupling agent of calcium carbonate crystal whisker 4%, 2% organic RE (carbonated rare earth), at 80 ℃ of lower 60min that stir, removes normal hexane;
3) with step 2) product that obtains adopts spray art to add weight in whipping process to be its organic acid of 0.3%, then at 80 ℃ of lower warm air drying 10h, to obtain function modified calcium carbonate crystal whisker.
Then, according to following prescription polypropylene and polyethylene are prepared burden with the pearl filler master batch: function modified calcium carbonate crystal whisker 60kg, vector resin (polyvinyl chloride) 16kg, coupling agent (silane coupling agent) 3kg, lubricant (ethylene bis stearic acid amide) 1kg.
At last, be prepared in accordance with the following steps polypropylene and polyethylene pearl filler master batch: function modified calcium carbonate crystal whisker is heated to 70 ℃, then add successively vector resin, coupling agent, lubricant stirs, and at 210 ℃ of lower 10min that keep, extruding pelletization obtains polypropylene and polyethylene pearl filler master batch.
Embodiment 4:
At first, prepare function modified calcium carbonate crystal whisker:
1) be that to place weight be that the water of 2 times of calcium carbonate crystal whiskers forms suspension liquid for the calcium carbonate crystal whisker of 1 μ m with diameter, adding weight in suspension liquid is the sodium stearate of calcium carbonate crystal whisker 1%, at 70 ℃ of lower 20min that stir, warm air drying also makes the water content of calcium carbonate crystal whisker＜1;
2) placing weight at the last product of step 1) is the normal hexane of 2 times of calcium carbonate crystal whiskers, and to add weight be the silane coupling agent of calcium carbonate crystal whisker 4%, 2% organic RE (rare earth hydrate), at 75 ℃ of lower 60min that stir, removes normal hexane;
3) with step 2) product that obtains adopts spray art to add weight in whipping process to be its organic acid of 0.3%, then at 80 ℃ of lower warm air drying 10h, to obtain function modified calcium carbonate crystal whisker.
Then, according to following prescription polypropylene and polyethylene are prepared burden with the pearl filler master batch: function modified calcium carbonate crystal whisker 60kg, vector resin (polyethylene) 16kg, coupling agent (titanate coupling agent) 3kg, lubricant (polyethylene wax) 1kg.
At last, be prepared in accordance with the following steps polypropylene and polyethylene pearl filler master batch: function modified calcium carbonate crystal whisker is heated to 70 ℃, then add successively vector resin, coupling agent, lubricant stirs, and at 210 ℃ of lower 10min that keep, extruding pelletization obtains polypropylene and polyethylene pearl filler master batch.
Claims (10)
1. a polypropylene and polyethylene pearl filler master batch, it is characterized in that, described polypropylene and polyethylene form with the raw material of pearl filler master batch each component by following parts by weight: function modified calcium carbonate crystal whisker 60-80 part, vector resin 10-20 part, coupling agent 0.5-3 part, lubricant 1-3 part.
2. polypropylene according to claim 1 and polyethylene pearl filler master batch is characterized in that, the diameter of described function modified calcium carbonate crystal whisker is 0.5-1 μ m.
3. polypropylene according to claim 1 and 2 and polyethylene pearl filler master batch is characterized in that, the preparation method of described function modified calcium carbonate crystal whisker is:
1) calcium carbonate crystal whisker being placed weight is that calcium carbonate crystal whisker 2-5 water doubly forms suspension liquid, adding weight in suspension liquid is the sodium stearate of calcium carbonate crystal whisker 0.3-2%, at the 50-80 ℃ of lower 20-40min that stirs, warm air drying also makes the water content of calcium carbonate crystal whisker＜1;
2) placing weight at the last product of step 1) is calcium carbonate crystal whisker 1-3 normal hexane doubly, and to add weight be the silane coupling agent of calcium carbonate crystal whisker 1-4%, the organic RE of 2-8%, at the 60-85 ℃ of lower 30-60min that stirs, removes normal hexane;
3) with step 2) product that obtains adopts spray art to add weight for the organic acid of its 0.3-1% in whipping process, then at 70-90 ℃ of lower warm air drying 5-10h, obtains function modified calcium carbonate crystal whisker.
4. polypropylene according to claim 3 and polyethylene pearl filler master batch is characterized in that, the temperature of described step 1) is 60-70 ℃.
5. polypropylene according to claim 3 and polyethylene pearl filler master batch is characterized in that, described step 2) organic RE be toxilic acid monoester rare earth, rare earth nitrate, carbonated rare earth, rare earth acetate or rare earth hydrate.
6. polypropylene according to claim 3 and polyethylene pearl filler master batch is characterized in that, described step 2) temperature be 75-80 ℃.
7. polypropylene according to claim 1 and 2 and polyethylene pearl filler master batch is characterized in that, described vector resin is polypropylene, polyethylene or polyvinyl chloride.
8. polypropylene according to claim 1 and 2 and polyethylene pearl filler master batch is characterized in that, described coupling agent is titanate coupling agent or silane coupling agent.
9. polypropylene according to claim 1 and 2 and polyethylene pearl filler master batch is characterized in that, described lubricant is polyethylene wax, stearic acid or ethylene bis stearic acid amide.
10. a polypropylene as claimed in claim 1 and polyethylene are with the preparation technology of pearl filler master batch, it is characterized in that, may further comprise the steps: be that the function modified calcium carbonate crystal whisker of 60-80 part is heated to 50-80 ℃ with parts by weight, then add successively vector resin 10-20 part, coupling agent 3-6 part, lubricant 1-3 part, stir, and at the 170-210 ℃ of lower 10-20min that keeps, extruding pelletization obtains polypropylene and polyethylene pearl filler master batch.
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| CN104231515A (en) * | 2014-09-11 | 2014-12-24 | 常州大学 | Anti-friction polypropylene material and preparation method thereof |
| CN104292649A (en) * | 2014-11-07 | 2015-01-21 | 合肥大安印刷有限责任公司 | Tough whisker sheet |
| CN106120321A (en) * | 2016-07-12 | 2016-11-16 | 江苏瑞科高新材料有限公司 | Calcium carbonate crystal whisker ginkgoic acid composite antibacterial fibre material and preparation method thereof |
| CN106675102A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Active calcium carbonate with environmental protection |
| CN106675108A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Environment-friendly activated calcium carbonate |
| CN106675101A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Environment-friendly active calcium carbonate |
| CN106675107A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Environmentally friendly active calcium carbonate |
| CN106675106A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Environment-friendly activated calcium carbonate |
| CN106675105A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Environmental-protection active calcium carbonate |
| CN106675103A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Environment-friendly activated calcium carbonate |
| CN106675104A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Environment-friendly active calcium carbonate |
| CN106675100A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Environment friendly active calcium carbonate |
| CN106675099A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Environmental-protection active calcium carbonate |
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| CN104231515A (en) * | 2014-09-11 | 2014-12-24 | 常州大学 | Anti-friction polypropylene material and preparation method thereof |
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| CN106675108A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Environment-friendly activated calcium carbonate |
| CN106675101A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Environment-friendly active calcium carbonate |
| CN106675107A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Environmentally friendly active calcium carbonate |
| CN106675106A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Environment-friendly activated calcium carbonate |
| CN106675099A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Environmental-protection active calcium carbonate |
| CN106675102A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Active calcium carbonate with environmental protection |
| CN106675104A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Environment-friendly active calcium carbonate |
| CN106675100A (en) * | 2015-11-05 | 2017-05-17 | 南通市永顺化工有限公司 | Environment friendly active calcium carbonate |
| CN106120321A (en) * | 2016-07-12 | 2016-11-16 | 江苏瑞科高新材料有限公司 | Calcium carbonate crystal whisker ginkgoic acid composite antibacterial fibre material and preparation method thereof |
| CN111004497A (en) * | 2019-12-24 | 2020-04-14 | 上海中镭新材料科技有限公司 | Electroplating nylon material and preparation method thereof |
| CN111004497B (en) * | 2019-12-24 | 2022-03-29 | 上海中镭新材料科技有限公司 | Electroplating nylon material and preparation method thereof |
| CN111978718A (en) * | 2020-07-31 | 2020-11-24 | 苏州新华美塑料有限公司 | High-performance nylon hub and preparation method thereof |
| CN114133729A (en) * | 2021-05-26 | 2022-03-04 | 国风塑业科技宿迁有限公司 | High-performance low-melting-point polyamide and preparation method thereof |
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