CN103131145A - Completely biodegradable stone paper material and preparation method thereof - Google Patents
Completely biodegradable stone paper material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a stone paper material, and in particular relates to a completely biodegradable stone paper material and a preparation method thereof. The completely biodegradable stone paper material is obtained by taking a completely biodegradable polymer as a carrier and adding a plasticizer, a bulking agent, a coupling reagent, a dispersing agent and inorganic filler. According to the completely biodegradable stone paper material, the problem that the existing stone paper taking traditional plastic polyethylene as the carrier is not biodegradable is solved, and the completely biodegradable stone paper material is completely biodegradable; and the preparation method is simple to operate and is easy to realize. The completely biodegradable stone paper material can be molded through blowing in a common low density polyethylene membrane blowing machine, the equipment does not need to be improved, the blowing process is simple, the cost is low, the equipment investment is low, and the completely biodegradable stone paper material is easy to popularize and apply.
Description
Technical field
The present invention relates to the stone paper material, be specifically related to a kind of complete biodegradable stone paper material and preparation method thereof.
Background technology
Now, paper has become a requisite part in people's life, it is widely used in again the fields such as wrapping material, sanitary material, environment protecting tableware as a kind of information recording carrier traditional, the most with the longest history, and China has become maximum paper product country of consumption.Along with improving constantly of rapid development of economy and people's living standard, people excessively use and depend on unduly paper, make people still increase year by year the demand of paper, thereby cause a large amount of trees to be cut down, add " three wastes " pollution problem of following in paper production, the integrated environment problem that causes is demanded a kind of new solution urgently.
Under such historical background, the stone paper material arises at the historic moment.Stone paper is mainly to dose the 70-80% ore powder with the 20-30% high molecular polymer to make.This paper need not water in whole production process, do not need to add strong acid, highly basic, chlorinated lime and numerous organic chloride, save several important pollution sections such as boiling, washing, bleaching than traditional paper technology, fundamentally stopped the pollution problem that causes because producing " three wastes " in the paper-making process; This paper is take cheap ore powder as main raw material(s), and cost is lower; Good waterproof performance; Grease proofing insect protected is good; Resistance to tearing, folding resistance are good; Good flame resistance; The oleophylic China ink is good, and the printing fastness is good; The ink-jet sharpness is high.
At present, a lot of about the report of stone paper, but seldom relevant for the report of biological degradation stone paper, and also the patent of report is all almost that conventional plastic polyethylene (PE) adds calcium carbonate and makes.
CN102180617A has reported a kind of biodegradable stone paper, but it forms still for PE adds calcium carbonate, even after the material disintegration fragmentates, PE is still the long-chain macromolecular structure on microtexture, be difficult to further be degraded into small molecules, more difficult degradation becomes carbonic acid gas and water.
CN102219949A has reported a kind of agricultural degradable stone paper and preparation method thereof, but its composition is difficult to realize real biological degradation still for PE adds calcium carbonate.
Summary of the invention
For existing stone paper take the conventional plastic polyethylene as carrier non-biodegradable problem, the purpose of this invention is to provide a kind of complete biodegradable stone paper material, this material can complete biodegradable; The present invention provides its preparation method simultaneously.
Complete biodegradable stone paper material of the present invention is that employing complete biodegradable polymkeric substance is carrier, by adding softening agent, expanding material, coupling agent, dispersion agent and mineral filler, obtains the stone paper material of complete biodegradable;
Described complete biodegradable polymkeric substance is one or more in following formula:
(1) aliphatic polyester that obtains of aliphatic dicarboxylic acid and aliphatic dihydroxy alcohol;
(2) aliphatic polyester that obtains of fatty alcohol acid compound;
(3) semi-aromatic polyester that obtains of aliphatic dicarboxylic acid, aromatic binary carboxylic acid and aliphatic dihydroxy alcohol.
The mass percent of this material consists of: complete biodegradable polymkeric substance 20-40%, softening agent 1-5%, expanding material 1-5%, coupling agent 1-5%, dispersion agent 1-5% and mineral filler 50-75%.
In order to guarantee stone paper material complete biodegradable, free from environmental pollution, we have selected the complete biodegradable resin is carrier, abandon original not biodegradable conventional plastic-polyethylene, after Biodegradable resin is resolved into carbonic acid gas and water fully by microorganism, ore powder is back to nature also, thereby reaches the purpose of real environmental protection.
Biodegradable material refers under physical environment and/or specific environment (soil, compost or seawater etc.), can be decomposed into the organic material such as carbonic acid gas and water fully by microorganism.at present, general biological degradation examination criteria is ASTMD6400 in the world, EN13432 and AS4736, resin by the biological degradation standard detection mainly contains poly butylene succinate (PBS), poly-succinic-hexanodioic acid-butanediol ester (PBSA), poly(lactic acid) (PLA), poly-hexane diacid-terephthalic acid-butylene terephthalate (PBAT), polycaprolactone (PCL), polyglycolic acid (PGA), poly-succinic-terephthalic acid-butanediol ester (PBST), polypropylene carbonate (PPC), poly-ethylene carbonate (PBC) and PHA series (poly butyric ester (PHB) for example, polyhydroxybutyrate-valerate (PHBV), polyhydroxybutyrate-capronate (PHBHX), poly-3, 4 hydroxybutyric acid ester (P3, 4-HB) etc.
Described complete biodegradable polymkeric substance is one or more in poly butylene succinate (PBS), poly-succinic-hexanodioic acid-butanediol ester (PBSA), poly(lactic acid) (PLA), poly-hexane diacid-terephthalic acid-butylene terephthalate (PBAT), polycaprolactone (PCL), polyglycolic acid (PGA), poly-succinic-terephthalic acid-butanediol ester (PBST), polypropylene carbonate (PPC), poly-ethylene carbonate (PBC) or PHA.
Described PHA is poly butyric ester (PHB), polyhydroxybutyrate-valerate (PHBV), polyhydroxybutyrate-capronate (PHBHX) or gathers 3,4 hydroxybutyric acid ester (P3,4-HB).
For complete biodegradable polymkeric substance and the relatively poor problem of ore powder consistency, we have taked the technique means such as special plasticising, increase-volume, coupling and dispersion, make a high proportion of mineral filler obtain well disperseing compatible with the interface in carrier.
Be generally irregular or spherical fine particle on the mineral filler microcosmic, specific surface area is large, and oil absorbency is high, easily reunite, be difficult to disperse in resin, therefore, introduce for example citric acid ester plasticizer in ore powder, can greatly reduce its specific surface area, improve its dispersiveness; In order further to improve its dispersiveness, can also add for example erucicamide class dispersion agent; By adding the compound of hydroxyl or carboxyl, form hydrogen bond action between carbonyl and mineral filler respectively and on resin, play compatibilization; By introducing titante coupling agent, further improve the interface interaction between resin and filler, improve consistency between the two.
Described softening agent is one or more the mixture in citric acid ester type (as tributyl citrate, trioctyl lemon acid, tributyl acetylcitrate, ATOC etc.), laurate class, cetylate class, stearate class (as glyceryl monostearate, glycerol stearate), ester gum, phthalate (as dioctyl phthalate (DOP) etc.), isophthalic acid ester class (as dioctyl isophthalate etc.).
Described expanding material is the compound that contains two or more hydroxyls and/or carboxyl, comprises one or more the mixture in ethylene glycol, propylene glycol, butyleneglycol, pentanediol, hexylene glycol, glycerine, oxalic acid, propanedioic acid, succinic acid, pentanedioic acid, oxysuccinic acid, hexanodioic acid, sebacic acid, terephthalic acid, m-phthalic acid, longer chain fatty acid (such as stearic acid, oleic acid, erucic acid etc.).
Described coupling agent is titante coupling agent, aluminate coupling agent, zirconate coupling agent or silane coupling agent.
Described dispersion agent is one or more the mixture in stearates (as calcium stearate, barium, zinc, magnesium etc.), organic carboxyl acid amides (as N, N-bis-stearamides, erucicamide, amine hydroxybenzene), wax class (as paraffin, polyethylene wax, oxidized polyethlene wax etc.) etc.
Described mineral filler is one or more the mixture in water-ground limestone, light calcium carbonate, talcum powder, mica powder, kaolin, polynite, sodium sulfate, barium sulfate, wollastonite, metal oxide (magnesium oxide, calcium oxide, aluminium sesquioxide, silicon-dioxide etc.), metal hydroxides (as aluminium hydroxide, magnesium hydroxide etc.), silicon whisker, and the fineness of described mineral filler is the 1250-2500 order.
Described complete biodegradable stone paper material preparation method is that each component is joined in the high-speed mixer that heats with oil bath, and under 20-80 ℃, 800-1400rpm stirs 30-240s, emits after preplasticizing; The preformed material is joined in the equidirectional parallel double-screw extruder of length-to-diameter ratio 〉=40 the stone paper material that further plasticizing extruding pelletization obtains a kind of complete biodegradable, extrusion temperature is 120-190 ℃ again.
Beneficial effect of the present invention is as follows:
The invention solves existing stone paper take the conventional plastic polyethylene as carrier non-biodegradable problem, this material can complete biodegradable; And the preparation method is simple, is easy to realize.
Complete biodegradable stone paper material of the present invention can blow molding on common Low Density Polyethylene (LDPE) inflation film manufacturing machine, need not equipment is transformed, and blow molding process is simple, and is with low cost, and equipment investment is little, is easy to apply.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
with 55% water-ground limestone (1250 order), 5% talcum powder (3000 order), 25%PBAT(fusing point: 110-120 ℃, the molten finger: 4.5), 5%PBS(fusing point: 114 ℃, the molten finger: 6.2), 3.5% tributyl acetylcitrate, 0.5% succinic acid, 1% 2 (dioctyl pyrophosphate) oxyacetate titanate (KR138S), 2%N, N-ethylene bis stearamide (EBS), 3%PE wax (fusing point: 95-100 ℃) joins in the high-speed mixer that heats with oil bath successively, oil bath temperature is set as 40 ° of C, (1400rpm) stirs 120s at a high speed, emit after preplasticizing, the preformed material is joined in length-to-diameter ratio 48 equidirectional parallel double-screw extruders further that the plasticizing extruding pelletization obtains the stone paper material, each district, forcing machine 12nd district is 120-140-145-150-150-150-150-150-150-145-145-140 ℃ again.
Embodiment 2
With 30% water-ground limestone (1250 order), 45% sodium sulfate (2000 order), 18%P3,4.3), 1% dioctyl phthalate (DOP), 1% glycerine, 2% γ-aminopropyl triethoxysilane (KH550), 1% erucicamide join in high-speed mixer with the oil bath heating successively 6.0), 2%PLA(fusing point: 160-170 ℃, the molten finger 4-HB(fusing point: 110-120 ℃, the molten finger::, oil bath temperature is set as 55 ℃, (1000rpm) stirs 80s at a high speed, emits after preplasticizing; The preformed material is joined in length-to-diameter ratio 48 equidirectional parallel double-screw extruders further that the plasticizing extruding pelletization obtains the stone paper material, it is 130-150-155-160-160-160-160-160-160-155-155-150 ℃ that forcing machine 12nd district respectively distinguish temperature again.
Embodiment 3
with 32% light calcium carbonate (3000 order), 20% mica powder (2000 order), 20%PBST(fusing point: 110-120 ℃, the molten finger: 3.0), 10%PBSA(fusing point: 85-95 ℃, the molten finger: 8.5), 5%PCL(is molten to be referred to: 23.1), 3.5% trioctyl lemon acid, 1.5% glyceryl monostearate, 0.5% oxysuccinic acid, 1% hexanodioic acid, 2.5% 3 (dodecyl benzenesulfonyl) isopropyl titanate (KR-9S), 1% calcium stearate, 3%N, N-bis-stearamides (EBS) joins in the high-speed mixer that heats with oil bath successively, oil bath temperature is set as 30 ℃, (800rpm) stirs 150s at a high speed, emit after preplasticizing, the preformed material is joined in length-to-diameter ratio 48 equidirectional parallel double-screw extruders further that the plasticizing extruding pelletization obtains the stone paper material, it is 110-120-130-130-130-130-130-130-130-130-125-120 ℃ that forcing machine 12nd district respectively distinguish temperature again.
Embodiment 4
12.5), 1.5% Laurate ethyl, 1% stearic acid, 0.8% erucic acid, 5% distearyl acyl-oxygen sec.-propyl Aluminate, 1% Magnesium Stearate, 0.7% oxidized polyethlene wax join in high-speed mixer with the oil bath heating successively 4.5), 8%PHBV(fusing point: 160-170 ℃, the molten finger with 25% magnesium oxide (1000 order), 25% barium sulfate (4000 order), 32%PBAT(fusing point: 110-120 ℃, the molten finger::, oil bath temperature is set as 60 ℃, (1200rpm) stirs 100s at a high speed, emits after preplasticizing; The preformed material is joined in length-to-diameter ratio 48 equidirectional parallel double-screw extruders further that the plasticizing extruding pelletization obtains the stone paper material, it is 120-140-145-150-150-150-150-150-150-145-145-140 ℃ that forcing machine 12nd district respectively distinguish temperature again.
Embodiment 5
10.7), 1.5% dioctyl isophthalate, 0.5% ester gum, 1% sebacic acid, 0.4% butyleneglycol, 2.6% 4 n-propyl zirconate, 0.5% amine hydroxybenzene, 1.5% paraffin (fusing point 60-65oC) join in high-speed mixer with the oil bath heating successively 4.5), 7%PPC(is molten refers to 30% water-ground limestone (1250 order), 15% light calcium carbonate (3000 order), 15% wollastonite (2000 order), 25%PBAT(fusing point: 110-120 ℃, the molten finger::, oil bath temperature is set as 60 ℃, (1200rpm) stirs 100s at a high speed, emits after preplasticizing; The preformed material is joined in length-to-diameter ratio 48 equidirectional parallel double-screw extruders further that the plasticizing extruding pelletization obtains the stone paper material, it is 120-140-145-150-150-150-150-150-150-145-145-140 ℃ that forcing machine 12nd district respectively distinguish temperature again.
(illustrate: moltenly in embodiment refer to that unit is g/10min, test condition: 190 ℃, 2.16kg.）
Claims (10)
1. complete biodegradable stone paper material is characterized in that: it is carrier that this material adopts complete biodegradable polymkeric substance, by adding softening agent, expanding material, coupling agent, dispersion agent and mineral filler, obtains the stone paper material of complete biodegradable;
Described complete biodegradable polymkeric substance is one or more in following formula:
(1) aliphatic polyester that obtains of aliphatic dicarboxylic acid and aliphatic dihydroxy alcohol;
(2) aliphatic polyester that obtains of fatty alcohol acid compound;
(3) semi-aromatic polyester that obtains of aliphatic dicarboxylic acid, aromatic binary carboxylic acid and aliphatic dihydroxy alcohol.
2. complete biodegradable stone paper material according to claim 1, is characterized in that the mass percent of this material consists of: complete biodegradable polymkeric substance 20-40%, softening agent 1-5%, expanding material 1-5%, coupling agent 1-5%, dispersion agent 1-5% and mineral filler 50-75%.
3. complete biodegradable stone paper material according to claim 1 and 2, is characterized in that the complete biodegradable polymkeric substance is one or more in poly butylene succinate, poly-succinic-hexanodioic acid-butanediol ester, poly(lactic acid), poly-hexane diacid-terephthalic acid-butylene terephthalate, polycaprolactone, polyglycolic acid, poly-succinic-terephthalic acid-butanediol ester, polypropylene carbonate, poly-ethylene carbonate or PHA.
4. complete biodegradable stone paper material according to claim 3, is characterized in that PHA is poly butyric ester, polyhydroxybutyrate-valerate, polyhydroxybutyrate-capronate or gathers 3, the 4 hydroxybutyric acid ester.
5. complete biodegradable stone paper material according to claim 1 and 2, is characterized in that softening agent is one or more in citric acid ester type, laurate class, cetylate class, stearate class, ester gum, phthalate, isophthalic acid ester class.
6. complete biodegradable stone paper material according to claim 1 and 2, is characterized in that expanding material is the compound that contains two or more hydroxyls and/or carboxyl.
7. complete biodegradable stone paper material according to claim 6, is characterized in that expanding material is one or more in ethylene glycol, propylene glycol, butyleneglycol, pentanediol, hexylene glycol, glycerine, oxalic acid, propanedioic acid, succinic acid, pentanedioic acid, oxysuccinic acid, hexanodioic acid, sebacic acid, terephthalic acid, m-phthalic acid, longer chain fatty acid.
8. complete biodegradable stone paper material according to claim 1 and 2, is characterized in that coupling agent is titante coupling agent, aluminate coupling agent, zirconate coupling agent or silane coupling agent; Dispersion agent is one or more in stearates, organic carboxyl acid amides or wax class.
9. complete biodegradable stone paper material according to claim 1 and 2, it is characterized in that mineral filler is one or more in water-ground limestone, light calcium carbonate, talcum powder, mica powder, kaolin, polynite, sodium sulfate, barium sulfate, wollastonite, magnesium oxide, calcium oxide, aluminium sesquioxide, silicon-dioxide, aluminium hydroxide, magnesium hydroxide or silicon whisker, the fineness of mineral filler is the 1250-2500 order.
10. complete biodegradable stone paper material preparation method claimed in claim 1 is characterized in that: each component is joined in high-speed mixer with the oil bath heating, and under 20-80 ℃, 800-1400rpm stirs 30-240s, emits after preplasticizing; The preformed material is joined in the equidirectional parallel double-screw extruder of length-to-diameter ratio 〉=40 the stone paper material that further plasticizing extruding pelletization obtains a kind of complete biodegradable, extrusion temperature is 120-190 ℃ again.
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| CN103980677A (en) * | 2014-05-16 | 2014-08-13 | 华中科技大学 | Preparation method of full-biodegradable rich mineral paper |
| CN104194289A (en) * | 2014-08-25 | 2014-12-10 | 浙江渤海卫生用品有限公司 | Bio-based biodegradable plastic bag material |
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| CN104693710A (en) * | 2015-03-23 | 2015-06-10 | 中山大学 | Biodegradable stone paper and preparation method thereof |
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