CN104356366B - A kind of wood powder modification makes the method for plastics - Google Patents
A kind of wood powder modification makes the method for plastics Download PDFInfo
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- CN104356366B CN104356366B CN201410598057.6A CN201410598057A CN104356366B CN 104356366 B CN104356366 B CN 104356366B CN 201410598057 A CN201410598057 A CN 201410598057A CN 104356366 B CN104356366 B CN 104356366B
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Abstract
The present invention relates to a kind of method that wood powder modification makes plastics, it adopts following steps: A) under normal temperature condition, first wood powder NaOH solution is washed, removing impurity, then vacuum filtration, washing wood powder is to neutral, air-dry under normal temperature, obtains Mierocrystalline cellulose; B) 6-caprolactone and Mierocrystalline cellulose are joined in Banbury mixer, and it is plumbous as catalyzer to add 2 ethyl hexanoic acid, keep rotor speed at 40-50 rpm, control temperature is on 120 DEG C, reaction times controls at 40-60min, obtain the cellulose product of 6-caprolactone graft modification, i.e. modified fibre plastics.C) by step B) in the product toluene Refining that obtains, and extract the complete 6-caprolactone of unreacted, and along the polycaprolactone homopolymer that band produces.D) by the modified fibre plastics product after the preliminary purification of step C gained with sodium hydroxide lye according to 1:80 deal ratio, extract product 22-26h, then by product vacuum-drying 3-5 days at 70-90 DEG C, obtain product.
Description
Technical field
The present invention relates to a kind of method that wood powder modification makes plastics, particularly a kind of graft modification with cellulose makes the method for degradable plastics.
Background technology
Along with the consumption of fossil energy, and the destruction that fossil energy product causes environment, a kind of eco-friendly degradable substitute products of exploitation are extremely urgent, and cellulose materials is a kind of biodegradable organic materials, can be degraded by microorganisms in physical environment.But Mierocrystalline cellulose is due to inner molecular structure own, its thermoplastic processability is poor.
Mierocrystalline cellulose is one of the abundantest renewable natural resource of occurring in nature, and Mierocrystalline cellulose has good hygroscopicity, antistatic, ventilation property is strong, and dyeing behavior is good, comfortable and easy to wear, be easy to textile process, can the premium properties such as biological degradation, have the advantages that man-made fiber hardly matches.Containing a large amount of hydroxyls in cellulosic molecule, be easy to be formed in molecule and intermolecular hydrogen bond, and decompose not melting under high temperature, but Mierocrystalline cellulose has good reactivity worth, its hydrogen bond is destroyed through chemical modification or graft reaction, just effectively can reduce fusing point, as multiple Industrial products, be widely used in the aspects such as weaving, membrane sepn, plastics, tobacco and coating.
In order to improve cellulosic thermoplastic processability, method of modifying more common at present carries out graft modification with derivatived cellulose, or etherificate, esterification, oxidation etc.But so just need multi-step process, not only loaded down with trivial details, and considerably increase production cost.
Summary of the invention
The object of the invention is the non-degradable for current plastic prod mostly on the market, environment caused to the problem of severe contamination, and provide a kind of with the wood powder fiber of cheapness for starting material, be modified as the working method of degradable plastics.The present invention is by the alkali cleaning in early stage to wood powder fiber, 6-caprolactone and cellulosic mixing, extraction and cleaning product, thus obtains degredation plastic product.
To achieve these goals, the technical solution used in the present invention is: a kind of wood powder modification makes the method for plastics, it is characterized in that adopting following steps:
A) under normal temperature condition, by mass fraction, it is first the NaOH solution washing of 8%-12% by 1-10 part wood powder 1-10 part mass percent concentration, removing pectin, xylogen and hemicellulose impurities, then vacuum filtration, washing wood powder is to neutral, and under normal temperature, air-dry 22-26h, obtains Mierocrystalline cellulose;
B) by mass fraction, by 1-10 part 6-caprolactone and steps A) in 1-10 part Mierocrystalline cellulose of obtaining join in Banbury mixer, in reaction, the massfraction of 6-caprolactone is 40-60%, and it is plumbous as catalyzer to add 1-5 part 2 ethyl hexanoic acid, keep rotor speed at 40-50 rpm, control temperature is on 120 DEG C, and the reaction times controls at 40-60min, obtain the cellulose product of 6-caprolactone graft modification, i.e. modified fibre plastics.
C) by mass fraction, by step B) in product 3-30 part toluene Refining of obtaining, and extract the complete 6-caprolactone of unreacted, and along the polycaprolactone homopolymer that band produces.
D) by the sodium hydroxide lye of the modified fibre plastics product after the preliminary purification of step C gained and mass percent concentration 10%-20% according to 1:80 deal ratio, extract product 22-26h, then by product vacuum-drying 3-5 days at 70-90 DEG C, product is obtained.
The invention has the beneficial effects as follows: 1) use cheap wood powder fiber to be raw material, wide material sources, simple.And operating process simple and convenient, just can carry out suitability for industrialized production, and product has, and easily degrades through simple modification environmentally friendly, the advantage of the low grade of cost.2) the present invention directly uses cellulosic raw material, directly processes, cost-saving, and enormously simplify manufacturing procedure.3) the plastic prod fusing point utilizing the inventive method obtained is low, is convenient to machine-shaping, and degradable, environmentally friendly, meets sustainable development view.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.Wood powder modification makes a method for plastics, and it adopts following steps:
A) under normal temperature condition, by mass fraction, it is first the NaOH solution washing of 8%-12% by 1-10 part wood powder 1-10 part mass percent concentration, removing pectin, xylogen and hemicellulose impurities, then vacuum filtration, washing wood powder is to neutral, and under normal temperature, air-dry 22-26h, obtains Mierocrystalline cellulose;
B) by mass fraction, by 1-10 part 6-caprolactone and steps A) in 1-10 part Mierocrystalline cellulose of obtaining join in Banbury mixer, in reaction, the massfraction of 6-caprolactone is 40-60%, and it is plumbous as catalyzer to add 1-5 part 2 ethyl hexanoic acid, keep rotor speed at 40-50 rpm, control temperature is on 120 DEG C, and the reaction times controls at 40-60min, obtain the cellulose product of 6-caprolactone graft modification, i.e. modified fibre plastics.
C) by mass fraction, by step B) in product 3-30 part toluene Refining of obtaining, and extract the complete 6-caprolactone of unreacted, and along the polycaprolactone homopolymer that band produces.
D) by the sodium hydroxide lye of the modified fibre plastics product after the preliminary purification of step C gained and mass percent concentration 10%-20% according to 1:80 deal ratio, extract product 22-26h, then by product vacuum-drying 3-5 days at 70-90 DEG C, product is obtained.
Protection scope of the present invention is not limited to following embodiment, and therefore, every technical scheme formed by simple numerical value replacement etc., is all formed specific embodiments of the invention, and form protection scope of the present invention.
Embodiment 1: a kind of wood powder modification makes the method for plastics, and it adopts following steps:
A) under normal temperature condition, by mass fraction, be first the NaOH solution washing of 8% with 1 part of mass percent concentration by 1 part of wood powder, removing pectin, xylogen and hemicellulose impurities, then vacuum filtration, washing wood powder is to neutral, under normal temperature air-dry 22, obtain Mierocrystalline cellulose;
B) by mass fraction, by 1 part of 6-caprolactone and steps A) in 1 part of Mierocrystalline cellulose obtaining join in Banbury mixer, in reaction, the massfraction of 6-caprolactone is 40%, and it is plumbous as catalyzer to add 1 part of 2 ethyl hexanoic acid, keep rotor speed at 40 rpms, control temperature is on 120 DEG C, and the reaction times controls at 40min, obtain the cellulose product of 6-caprolactone graft modification, i.e. modified fibre plastics.
C) by mass fraction, by step B) in product 3 parts of toluene Refinings of obtaining, and extract the complete 6-caprolactone of unreacted, and along the polycaprolactone homopolymer that band produces.
D) by the sodium hydroxide lye of the modified fibre plastics product after the preliminary purification of step C gained and mass percent concentration 10% according to 1:80 deal ratio, extract product 22h, then by product vacuum-drying 3 days at 70 DEG C, obtain product.
Embodiment 2: a kind of wood powder modification makes the method for plastics, and it adopts following steps:
A) under normal temperature condition, by mass fraction, be first the NaOH solution washing of 10% with 5 parts of mass percent concentrations by 5 parts of wood powders, removing pectin, xylogen and hemicellulose impurities, then vacuum filtration, washing wood powder is to neutral, under normal temperature, air-dry 24h, obtains Mierocrystalline cellulose;
B) by mass fraction, by 5 parts of 6-caprolactones and steps A) in 5 parts of Mierocrystalline celluloses obtaining join in Banbury mixer, in reaction, the massfraction of 6-caprolactone is 50%, and it is plumbous as catalyzer to add 3 parts of 2 ethyl hexanoic acids, keep rotor speed at 45 rpms, control temperature is on 120 DEG C, and the reaction times controls at 50min, obtain the cellulose product of 6-caprolactone graft modification, i.e. modified fibre plastics.
C) by mass fraction, by step B) in product 10 parts of toluene Refinings of obtaining, and extract the complete 6-caprolactone of unreacted, and along the polycaprolactone homopolymer that band produces.
D) by the sodium hydroxide lye of the modified fibre plastics product after the preliminary purification of step C gained and mass percent concentration 15% according to 1:80 deal ratio, extract product 24h, then by product vacuum-drying 4 days at 80 DEG C, obtain product.
Embodiment 3: a kind of wood powder modification makes the method for plastics, and it adopts following steps:
A) under normal temperature condition, by mass fraction, be first the NaOH solution washing of 12% with 10 parts of mass percent concentrations by 10 parts of wood powders, removing pectin, xylogen and hemicellulose impurities, then vacuum filtration, washing wood powder is to neutral, under normal temperature, air-dry 26h, obtains Mierocrystalline cellulose;
B) by mass fraction, by 10 parts of 6-caprolactones and steps A) in 10 parts of Mierocrystalline celluloses obtaining join in Banbury mixer, in reaction, the massfraction of 6-caprolactone is 60%, and it is plumbous as catalyzer to add 5 parts of 2 ethyl hexanoic acids, keep rotor speed at 50 rpms, control temperature is on 120 DEG C, and the reaction times controls at 60min, obtain the cellulose product of 6-caprolactone graft modification, i.e. modified fibre plastics.
C) by mass fraction, by step B) in product 20 parts of toluene Refinings of obtaining, and extract the complete 6-caprolactone of unreacted, and along the polycaprolactone homopolymer that band produces.
D) by the sodium hydroxide lye of the modified fibre plastics product after the preliminary purification of step C gained and mass percent concentration 20% according to 1:80 deal ratio, extract product 26h, then by product vacuum-drying 5 days at 90 DEG C, obtain product.
Embodiment 4: a kind of wood powder modification makes the method for plastics, and it adopts following steps:
A) under normal temperature condition, by mass fraction, be first the NaOH solution washing of 12% with 10 parts of mass percent concentrations by 10 parts of wood powders, removing pectin, xylogen and hemicellulose impurities, then vacuum filtration, washing wood powder is to neutral, under normal temperature, air-dry 26h, obtains Mierocrystalline cellulose;
B) by mass fraction, by 10 parts of 6-caprolactones and steps A) in 10 parts of Mierocrystalline celluloses obtaining join in Banbury mixer, in reaction, the massfraction of 6-caprolactone is 60%, and it is plumbous as catalyzer to add 5 parts of 2 ethyl hexanoic acids, keep rotor speed at 50 rpms, control temperature is on 120 DEG C, and the reaction times controls at 60min, obtain the cellulose product of 6-caprolactone graft modification, i.e. modified fibre plastics.
C) by mass fraction, by step B) in product 30 parts of toluene Refinings of obtaining, and extract the complete 6-caprolactone of unreacted, and along the polycaprolactone homopolymer that band produces.
D) by the sodium hydroxide lye of the modified fibre plastics product after the preliminary purification of step C gained and mass percent concentration 15% according to 1:80 deal ratio, extract product 26h, then by product vacuum-drying 5 days at 85 DEG C, obtain product.
Claims (2)
1. wood powder modification makes a method for plastics, it is characterized in that adopting following steps:
A) under normal temperature condition, by mass fraction, be first the NaOH solution washing of 8%-12% by 1-10 part wood powder 1-10 part mass percent concentration, removing pectin, xylogen and hemicellulose impurities, then vacuum filtration, washing wood powder is to neutral, under normal temperature, air-dry 22-26h, obtains Mierocrystalline cellulose;
B) by mass fraction, by 1-10 part 6-caprolactone and steps A) in 1-10 part Mierocrystalline cellulose of obtaining join in Banbury mixer, in reaction, the massfraction of 6-caprolactone is 40-60%, and it is plumbous as catalyzer to add 1-5 part 2 ethyl hexanoic acid, keep rotor speed at 40-50 rpm, control temperature is on 120 DEG C, and the reaction times controls at 40-60min, obtain the cellulose product of 6-caprolactone graft modification, i.e. modified fibre plastics;
C) by mass fraction, by step B) in product 3-30 part toluene Refining of obtaining, and extract the complete 6-caprolactone of unreacted, and along the polycaprolactone homopolymer that band produces;
D) by the sodium hydroxide lye of the modified fibre plastics product after the preliminary purification of step C gained and mass percent concentration 10%-20% according to 1:80 deal ratio, extract product 22-26h, then by product vacuum-drying 3-5 days at 70-90 DEG C, product is obtained.
2. wood powder modification makes a method for plastics, it is characterized in that it adopts following steps:
A) under normal temperature condition, by mass fraction, be first the NaOH solution washing of 10% with 5 parts of mass percent concentrations by 5 parts of wood powders, removing pectin, xylogen and hemicellulose impurities, then vacuum filtration, washing wood powder is to neutral, under normal temperature, air-dry 24h, obtains Mierocrystalline cellulose;
B) by mass fraction; by 5 parts of 6-caprolactones and steps A) in 5 parts of Mierocrystalline celluloses obtaining join in Banbury mixer; in reaction, the massfraction of 6-caprolactone is 50%; and it is plumbous as catalyzer to add 3 parts of 2 ethyl hexanoic acids; keep rotor speed at 45 rpms, control temperature is on 120 DEG C, and the reaction times controls at 50min; obtain the cellulose product of 6-caprolactone graft modification, i.e. modified fibre plastics;
C) by mass fraction, by step B) in product 10 parts of toluene Refinings of obtaining, and extract the complete 6-caprolactone of unreacted, and along the polycaprolactone homopolymer that band produces;
D) by the sodium hydroxide lye of the modified fibre plastics product after the preliminary purification of step C gained and mass percent concentration 15% according to 1:80 deal ratio, extract product 24h, then by product vacuum-drying 4 days at 80 DEG C, obtain product.
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| CN1152007A (en) * | 1995-09-26 | 1997-06-18 | 拜尔公司 | Biodegradable plastics filled with reinforcing materials |
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| CN1152007A (en) * | 1995-09-26 | 1997-06-18 | 拜尔公司 | Biodegradable plastics filled with reinforcing materials |
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Effective date of registration: 20200622 Address after: 546700, the Guangxi Zhuang Autonomous Region Wuzhou Mengshan County Industrial Concentration Zone Tung Oil flat area Patentee after: Guangxi Qingmiao New Material Co., Ltd Address before: 310018 No. 2, Xiasha Higher Education Zone, Hangzhou, Zhejiang Patentee before: ZHEJIANG SCI-TECH University |
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Effective date of registration: 20200817 Address after: No. 32, No. 3 Road, Wuzhou Industrial Park, 543000 Guangxi Zhuang Autonomous Region Patentee after: GUANGXI SHASHADAO INDUSTRIAL Co.,Ltd. Address before: 546700, the Guangxi Zhuang Autonomous Region Wuzhou Mengshan County Industrial Concentration Zone Tung Oil flat area Patentee before: Guangxi Qingmiao New Material Co., Ltd |