CN109370192A - A kind of lignin enhancing pc material and preparation method thereof - Google Patents
A kind of lignin enhancing pc material and preparation method thereof Download PDFInfo
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- CN109370192A CN109370192A CN201811188837.8A CN201811188837A CN109370192A CN 109370192 A CN109370192 A CN 109370192A CN 201811188837 A CN201811188837 A CN 201811188837A CN 109370192 A CN109370192 A CN 109370192A
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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
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
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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
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/06—Polymer mixtures characterised by other features having improved processability or containing aids for moulding methods
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Compounds Of Unknown Constitution (AREA)
Abstract
The invention discloses a kind of lignin to enhance pc material, it is composed of the following raw materials by weight: calcium oxide 3-4, polycarbonate 100-120, dioctyl sebacate 5-7, carbon nanotube 20-30, lignin 10-13, p-methyl benzenesulfonic acid 2-4, acid binding agent 0.01-0.02, sodium sulfite 2-3, the present invention improves the dispersion compatibility of lignin, carbon nanotube between polycarbonate, to improve the mechanical stability and intensity of finished-product material, lignin is effectively distributed in polycarbonate by the present invention, effectively raises the toughness of finished product.
Description
Technical field
The invention belongs to Material Fields, and in particular to a kind of lignin enhancing pc material and preparation method thereof.
Background technique
Polycarbonate (PC) is the synthesis macromolecule in strand containing carbonate group.Not according to R group in strand
Together, polycarbonate can be divided into aliphatic, aromatic series, alicyclic and four major class of aliphatic-aromatic race.Wherein aliphatic poly carbon
Acid esters cannot function as engineering plastics use, aliphatic-aromatic race and alicyclic ring since mechanical strength is poor, fusing point is low, thermal stability is poor
Though race is higher than aliphatic fusing point, requirement is still not achieved in its mechanical strength, therefore really with industrial application value
There is aromatic copolycarbonate；Benzene ring structure containing rigidity in polycarbonate structural units, limits the interior rotation of strand, point
The flexibility of subchain reduces, thus PC glass transition temperature with higher (Tg=145~149 DEG C), higher viscosity flow temperature
It spends (Tf=215~225 DEG C), rigid benzene ring structure makes it, and deformation quantity is small under by external force, and product size is stablized.Rigid phenyl ring
With ester group structure more flexible, the excellent tensile strength of PC, high impact toughness at room temperature and low water absorption are imparted.PC's is upper
The a variety of excellent properties stating structure and being determined by structure, make it in electronic apparatus, traffic, building, aviation, agricultural, medical treatment, spinning
It the every profession and trades such as knits all to be widely used；
In practical applications, PC there are still some drawbacks.Rigid benzene ring structure limits the orientation of PC molecule interchain, by
To after external force, orientation is not easy to relax, and strand residualinternal stress is difficult to eliminate, and internal stress is frozen, holds PC product
The phenomenon that being also easy to produce stress cracking, therefore, the toughness and intensity for how improving pc are the emphasis studied at present.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of lignin enhancing pc material and its
Preparation method.
To achieve the above object, the invention adopts the following technical scheme:
A kind of lignin enhancing pc material, it is composed of the following raw materials by weight:
Calcium oxide 3-4, polycarbonate 100-120, dioctyl sebacate 5-7, carbon nanotube 20-30, lignin 10-13,
P-methyl benzenesulfonic acid 2-4, acid binding agent 0.01-0.02, sodium sulfite 2-3.
The acid binding agent is triethylamine.
A kind of preparation method of lignin enhancing pc material, comprising the following steps:
(1) carbon nanotube is taken, in nitric acid solution that be added to 20-30 times of its weight, 96-98%, ultrasonic 10-15 is small
When, precipitating is washed in filtering, and air drying is mixed with p-methyl benzenesulfonic acid, and increasing temperature is 60-70 DEG C, insulated and stirred 30-
40 minutes, the thionyl chloride of 2-3 times of mixture weight is added, it is 1-2 hours ultrasonic, thionyl chloride is distilled off, obtains chloride carbon
Nanotube；
(2) lignin, sodium sulfite mixing are taken, is added in the deionized water of 10-13 times of mixture weight, increases temperature
It is 70-80 DEG C, insulated and stirred 1-2 hours, calcium oxide is added, is sent in baking oven, dry to constant weight, discharging cooling must activates
Lignin；
(3) 13-20% for taking polycarbonate weight is added in the toluene of 4-6 times of its weight, stirs evenly, and addition is tied up
Sour agent, increasing temperature is 50-60 DEG C, insulated and stirred 1-2 hours, obtains polycarbonate dispersion liquid；
(4) above-mentioned acyl chlorides carbon nano tube, activation lignin mixing are taken, is added in polycarbonate dispersion liquid, stirring is equal
It is even, it is sent in reaction kettle, is passed through nitrogen, reacted 6-10 hours at 3-5 DEG C, discharged, revolving removing toluene, air drying,
Polyester must be pre-processed；
(5) above-mentioned pretreatment polyester is taken, mixes, stirs evenly with remaining polycarbonate, dioctyl sebacate, be sent to
In extruder, melting extrusion is cooling to enhance pc material to get the lignin.
Advantages of the present invention:
The present invention is first handled carbon nanotube using after acid activation by thionyl chloride, obtains the carbon nanometer of chloride
Pipe, then lignin is activated, is blended with acyl chlorides carbon nano tube, using the toluene solution of polycarbonate as reaction dissolvent, pass through
Phenolic hydroxyl group and acyl chlorides react in lignin, improve the dispersion compatibility of lignin, carbon nanotube between polycarbonate, thus
The mechanical stability and intensity of finished-product material are improved, lignin is effectively distributed in polycarbonate by the present invention, effectively
Improve the toughness of finished product.
Specific embodiment
Embodiment 1
A kind of lignin enhancing pc material, it is composed of the following raw materials by weight:
Calcium oxide 4, polycarbonate 120, dioctyl sebacate 7, carbon nanotube 30, lignin 13, p-methyl benzenesulfonic acid 4,
Acid binding agent 0.02, sodium sulfite 3.
The acid binding agent is triethylamine.
A kind of preparation method of lignin enhancing pc material, comprising the following steps:
(1) carbon nanotube is taken, is added in 30 times of its weight, 98% nitric acid solution, ultrasound 15 hours filters, will
Precipitating washing, air drying are mixed with p-methyl benzenesulfonic acid, and increasing temperature is 70 DEG C, and insulated and stirred 40 minutes, mixture is added
The thionyl chloride that 3 times of weight, ultrasound 2 hours, is distilled off thionyl chloride, obtains acyl chlorides carbon nano tube；
(2) lignin, sodium sulfite mixing are taken, is added in 13 times of mixture weight of deionized water, increasing temperature is
80 DEG C, insulated and stirred 2 hours, calcium oxide is added, is sent in baking oven, dry to constant weight, discharging cooling obtains activation lignin；
(3) the 20% of polycarbonate weight is taken, is added in the toluene of 6 times of its weight, stirs evenly, acid binding agent is added,
Increasing temperature is 60 DEG C, insulated and stirred 2 hours, obtains polycarbonate dispersion liquid；
(4) above-mentioned acyl chlorides carbon nano tube, activation lignin mixing are taken, is added in polycarbonate dispersion liquid, stirring is equal
It is even, it is sent in reaction kettle, is passed through nitrogen, react 10 hours at 5 DEG C, discharging, revolving removes toluene, and air drying obtains pre-
Handle polyester；
(5) above-mentioned pretreatment polyester is taken, mixes, stirs evenly with remaining polycarbonate, dioctyl sebacate, be sent to
In extruder, melting extrusion is cooling to enhance pc material to get the lignin.
Embodiment 2
A kind of lignin enhancing pc material, it is composed of the following raw materials by weight:
Calcium oxide 3, polycarbonate 100, dioctyl sebacate 5, carbon nanotube 20, lignin 10, p-methyl benzenesulfonic acid 2,
Acid binding agent 0.01, sodium sulfite 2.
The acid binding agent is triethylamine.
A kind of preparation method of lignin enhancing pc material, comprising the following steps:
(1) carbon nanotube is taken, is added in 20 times of its weight, 96% nitric acid solution, ultrasound 10 hours filters, will
Precipitating washing, air drying are mixed with p-methyl benzenesulfonic acid, and increasing temperature is 60 DEG C, and insulated and stirred 30 minutes, mixture is added
The thionyl chloride that 2 times of weight, ultrasound 1 hour, is distilled off thionyl chloride, obtains acyl chlorides carbon nano tube；
(2) lignin, sodium sulfite mixing are taken, is added in 10 times of mixture weight of deionized water, increasing temperature is
70 DEG C, insulated and stirred 1 hour, calcium oxide is added, is sent in baking oven, dry to constant weight, discharging cooling obtains activation lignin；
(3) the 13% of polycarbonate weight is taken, is added in the toluene of 4 times of its weight, stirs evenly, acid binding agent is added,
Increasing temperature is 50 DEG C, insulated and stirred 1 hour, obtains polycarbonate dispersion liquid；
(4) above-mentioned acyl chlorides carbon nano tube, activation lignin mixing are taken, is added in polycarbonate dispersion liquid, stirring is equal
It is even, it is sent in reaction kettle, is passed through nitrogen, reacted 6 hours at 3 DEG C, discharged, revolving removes toluene, and air drying obtains pre- place
Manage polyester；
(5) above-mentioned pretreatment polyester is taken, mixes, stirs evenly with remaining polycarbonate, dioctyl sebacate, be sent to
In extruder, melting extrusion is cooling to enhance pc material to get the lignin.
Impact property test, according to standard GB/T1043-1993, using Charpy impact machine tester, test material is -50
DEG C notch impact strength, batten is having a size of 63mm × 12.7mm × 4mm, notch depth 2.54mm, shock loading 5.4J；
It impacts batten and after placement 5h, takes out test immediately, entire shock-testing process is in 10s in low-temperature impact test slot (- 50 DEG C)
Interior completion；
It measures；
The impact strength of the lignin enhancing pc material of the embodiment of the present invention 1 is 63.1kJ/m2；
The impact strength of the lignin enhancing pc material of the embodiment of the present invention 2 is 64.7kJ/m2；
The impact strength of commercially available pc material is 10.7kJ/m2。
Claims (3)
1. a kind of lignin enhances pc material, which is characterized in that it is composed of the following raw materials by weight:
Calcium oxide 3-4, polycarbonate 100-120, dioctyl sebacate 5-7, carbon nanotube 20-30, lignin 10-13, to first
Base benzene sulfonic acid 2-4, acid binding agent 0.01-0.02, sodium sulfite 2-3.
2. a kind of lignin according to claim 1 enhances pc material, which is characterized in that the acid binding agent is three second
Amine.
3. a kind of preparation method of lignin enhancing pc material as described in claim 1, which comprises the following steps:
(1) carbon nanotube is taken, 10-15 hours ultrasonic in nitric acid solution that be added to 20-30 times of its weight, 96-98%, mistake
Precipitating is washed in filter, and air drying is mixed with p-methyl benzenesulfonic acid, and increasing temperature is 60-70 DEG C, insulated and stirred 30-40 points
The thionyl chloride of 2-3 times of mixture weight is added in clock, 1-2 hours ultrasonic, and thionyl chloride is distilled off, obtains chloride carbon nanometer
Pipe；
(2) lignin, sodium sulfite mixing are taken, is added in the deionized water of 10-13 times of mixture weight, increasing temperature is
70-80 DEG C, insulated and stirred 1-2 hours, calcium oxide is added, is sent in baking oven, dry to constant weight, discharging cooling must activate wood
Quality；
(3) 13-20% for taking polycarbonate weight is added in the toluene of 4-6 times of its weight, stirs evenly, and acid binding agent is added,
Increasing temperature is 50-60 DEG C, insulated and stirred 1-2 hours, obtains polycarbonate dispersion liquid；
(4) above-mentioned acyl chlorides carbon nano tube, activation lignin mixing are taken, is added in polycarbonate dispersion liquid, stirs evenly, send
Enter into reaction kettle, be passed through nitrogen, reacted 6-10 hours at 3-5 DEG C, discharged, revolving removes toluene, and air drying obtains pre- place
Manage polyester；
(5) above-mentioned pretreatment polyester is taken, mixes, stirs evenly with remaining polycarbonate, dioctyl sebacate, is sent to extrusion
In machine, melting extrusion is cooling to enhance pc material to get the lignin.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811188837.8A CN109370192A (en) | 2018-10-12 | 2018-10-12 | A kind of lignin enhancing pc material and preparation method thereof |
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| CN201811188837.8A CN109370192A (en) | 2018-10-12 | 2018-10-12 | A kind of lignin enhancing pc material and preparation method thereof |
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| CN104016341A (en) * | 2014-07-01 | 2014-09-03 | 济南圣泉集团股份有限公司 | Preparation method of porous graphene |
| US20160002467A1 (en) * | 2013-02-11 | 2016-01-07 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Thermoplastic polymer compounds with low-molecular lignins, method for the production thereof, moulded articles and also uses |
| CN106632916A (en) * | 2016-12-15 | 2017-05-10 | 安徽华宇管道制造有限公司 | Anticorrosion grafted composite elastic material and preparation method thereof |
| CN106752007A (en) * | 2016-12-25 | 2017-05-31 | 符英 | Poly (propylene carbonate)/agricultural-forestry biomass composite, Preparation method and use |
-
2018
- 2018-10-12 CN CN201811188837.8A patent/CN109370192A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160002467A1 (en) * | 2013-02-11 | 2016-01-07 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Thermoplastic polymer compounds with low-molecular lignins, method for the production thereof, moulded articles and also uses |
| CN104016341A (en) * | 2014-07-01 | 2014-09-03 | 济南圣泉集团股份有限公司 | Preparation method of porous graphene |
| CN106632916A (en) * | 2016-12-15 | 2017-05-10 | 安徽华宇管道制造有限公司 | Anticorrosion grafted composite elastic material and preparation method thereof |
| CN106752007A (en) * | 2016-12-25 | 2017-05-31 | 符英 | Poly (propylene carbonate)/agricultural-forestry biomass composite, Preparation method and use |
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Application publication date: 20190222 |