CN101831001B - Method for preparing konjak glucomannan acetate thermoplastic material - Google Patents

Method for preparing konjak glucomannan acetate thermoplastic material Download PDF

Info

Publication number
CN101831001B
CN101831001B CN 201010177363 CN201010177363A CN101831001B CN 101831001 B CN101831001 B CN 101831001B CN 201010177363 CN201010177363 CN 201010177363 CN 201010177363 A CN201010177363 A CN 201010177363A CN 101831001 B CN101831001 B CN 101831001B
Authority
CN
China
Prior art keywords
glucomannan
konjak glucomannan
rhizoma amorphophalli
konjak
swelling
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN 201010177363
Other languages
Chinese (zh)
Other versions
CN101831001A (en
Inventor
林晓艳
吴强
罗学刚
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Southwest University of Science and Technology
Original Assignee
Southwest University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Southwest University of Science and Technology filed Critical Southwest University of Science and Technology
Priority to CN 201010177363 priority Critical patent/CN101831001B/en
Publication of CN101831001A publication Critical patent/CN101831001A/en
Application granted granted Critical
Publication of CN101831001B publication Critical patent/CN101831001B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Abstract

The invention discloses a method for preparing a konjak glucomannan acetate thermoplastic material, which is characterized by comprising the following steps of: adding 1 to 30 weight parts of purified konjak glucomannan into 50 to 300 weight parts of swelling control agent, stirring the mixture for 1 to 10 hours at the temperature of between 25 and 80 DEG C and then filtering the mixture, mixing the swelled konjak glucomannan and 100 to 300 weight parts of dispersant and stirring the mixture for 10 to 50 minutes, then adding 50 to 300 weight parts of acetic anhydride and 0.001 to 0.1 weight part of catalyst into the mixture, and reacting the mixture for 0.1 to 5 hours at the temperature of between 30 and 95 DEG C to obtain solution after the esterification reaction of the konjak glucomannan; and cooling the solution, adding water into the solution to separate out sediment, filtering the solution, washing the sediment, and then drying the sediment to obtain the konjak glucomannan acetate thermoplastic material. The material has good thermoplastic property, can be used as a thermoplastic filling material and a blending material, is processed and shaped by using the traditional extrusion molding, injection molding or blow molding method, and is subjected to scale processing and production.

Description

A kind of preparation method of konjak glucomannan acetate thermoplastic material
Technical field
The invention belongs to the preparation method of konjac glucomanna derivative, relate to a kind of preparation method of konjak glucomannan acetate thermoplastic material, is the preparation method of the ecological environment material nd in a kind of novel material.The konjak glucomannan acetate thermoplastic material of the inventive method preparation has good thermoplastic, can be used as thermoplastic packing material, intermingling material, and mass-producing processing and production are carried out in available traditional extrusion molding, injection moulding, blow moiding method machine-shaping; Degrade fully and environmental friendliness after its goods use, can be widely used in fields such as chemical industry, food, medicine, agricultural, packing and environmental protection.
Background technology
It is exhausted day by day and use and bring serious environmental to pollute two hang-ups after discarded to be with oil, Sweet natural gas that the synthesized polymer material of raw material is faced with raw material.The effective way that solves this two hang-up is to seek a kind of aboundresources, renewable, degradable natural macromolecular material, it is carried out modifications such as physical chemistry, production can be satisfied the eco-friendly polymer novel material of service requirements, reduction reduces material and uses the pollution of back to environment the consumption of limited resources.Rhizoma amorphophalli glucomannan is that a kind of source is abundant, renewable, degradable natural polymer, can prepare degradative plastics goods as raw material with wide application prospect, but there is a large amount of hydroxyls on the Rhizoma amorphophalli glucomannan molecular chain, intermolecular and intramolecularly has very strong hydrogen bond action, be difficult to motion between the molecule segment, thereby the temperature that has caused the second-order transition temperature of Rhizoma amorphophalli glucomannan and heating and melting is far above its decomposition temperature, make it not have thermoplasticity, can not directly plastify processing with the conventional plastic processing units, maybe need use special processing units, this will cause tooling cost to increase.Can not carry out the polyblend that the melt blending acquisition has specific function as the simple adding softening agent of starch or other polymer.Therefore, need carry out the thermoplasticity modification, improve its processing characteristics, be convenient to carry out mass-producing processing and production, widen its range of application with traditional thermoplastic processing to Rhizoma amorphophalli glucomannan.
Polysaccharide is the abundantest natural polymer of nature, it is wide to have the source, renewable, advantages such as degradable, polysaccharide is applied to polymeric material field, to solve two hang-ups that present synthesized polymer material field faces: petroleum resources shortage and synthetic macromolecule use " white pollution " that brings after discarded, therefore develop natural macromolecule amylose, for save petroleum resources, reduce white pollution, realization Sustainable development etc. is significant.
The thermoplasticity modification of starch-polysaccharides has a large amount of research, and the material modified example that comes into operation of existing starch base thermoplastic, Rhizoma amorphophalli glucomannan is after Mierocrystalline cellulose and starch, the renewable natural macromolecule amylose that another source is abundant, has biodegradable, the molecular weight advantages of higher, at food, medicine, chemical industry, weaving, printing and dyeing, papermaking, oil, each production field such as geology has purposes widely, has become China central and west regions and has adjusted the structure of agricultural production, peasant programme, one of mainstay industry of foreign exchange earning and increase local finance.But the thermoplastic study on the modification of Rhizoma amorphophalli glucomannan is less, and the modification of graft copolymerization thermoplastic is only arranged, with polymer blended thermoplastic modification, the modification of etherificate thermoplastic and the rarely seen report of esterification thermoplastic modification.Konjaku is the local product resource of China, Rhizoma amorphophalli glucomannan as important composition in the konjaku is a kind of natural macromolecule amylose, therefore, Rhizoma amorphophalli glucomannan is carried out physical chemistry thermoplastic study on the modification, being convenient to will have crucial practical significance with traditional thermoplastic processing units and method processing.
Summary of the invention
Purpose of the present invention is intended to overcome above-mentioned deficiency of the prior art, and a kind of preparation method of eco-friendly konjak glucomannan acetate thermoplastic material is provided, thereby provides an effective way for the mass-producing of renewable resources Rhizoma amorphophalli glucomannan development and use.
Content of the present invention is: a kind of preparation method of konjak glucomannan acetate thermoplastic material is characterized in that comprising the following steps:
A, Rhizoma amorphophalli glucomannan swelling: the purifying Rhizoma amorphophalli glucomannan of 1~30 weight part is joined in the swelling control agent of 50~300 weight parts, under 25~80 ℃ temperature, stir 1~10 hour after-filtration of swelling, the swollen Rhizoma amorphophalli glucomannan;
Described purifying Rhizoma amorphophalli glucomannan is the konjac glucomanna that extracts from the plant konjaku, (can be again through ethanolic soln purify, median size be 1~100um), the weight percentage of konjac glucomanna 〉=50~80% wherein;
Described swelling control agent is that concentration of volume percent is a kind of in water (for the solvent) solution of 10~80% methyl alcohol, ethanol or acetone;
B, preparation konjak glucomannan acetate: the dispersant of swollen Rhizoma amorphophalli glucomannan and 100~300 weight parts was stirred 10~50 minutes, add the acetic anhydride of 50~300 weight parts, the catalyzer of 0.001~0.1 weight part again, under 30~95 ℃ temperature, reacted 0.1~5 hour, and obtained the konjak glucomannan esters reacted solution;
Described dispersion agent is a Glacial acetic acid;
Described catalyzer is methylsulphonic acid (a namely for methane sulfonic acid);
C, with konjak glucomannan esters reacted solution cooling (to room temperature), add 3~10 times of described liquor capacities water, separate out (white) precipitation, filter, after the each water with 3~10 times of volumes of solids washs 1-3 time altogether, in 30~90 ℃ of dryings 5~30 hours, promptly make the cotton-shaped hydrophobic konjak glucomannan acetate thermoplastic material of white loose.
In the content of the present invention: described dispersion agent can also replace with a kind of in acetone, the dimethyl sulfoxide (DMSO).
In the content of the present invention: it is 98% the vitriol oil that described catalyzer can also replace with picoline, weight percentage, cross a kind of in the inorganic or organic acid such as chloric acid, methylsulfonic acid, methyl disulfonic acid, Witco 1298 Soft Acid or iron(ic) chloride.
Preparation method's of the present invention reaction mechanism:
Figure GSA00000107822600031
Preparation method's synthetic konjak glucomannan acetate thermoplastic material of the present invention is the cotton-shaped solid of white loose, and its density is 0.8~1.2g/cm 3The thermoplastic materials substitution value is 0.5~3, water-intake rate is 1~8%, it is typical viscous-elastic material, its second-order transition temperature (Tg) is 120~200 ℃, has good thermoplastic, can be used as thermoplastic packing material, intermingling material, mass-producing processing and production are carried out in available traditional extrusion molding, injection moulding, blow moiding method machine-shaping; The elongation at break of its goods is 20~35%, tensile strength is that 5~10MPa, shock strength are 2~5KJ/m 2, and degrade fully and environmental friendliness after using, can be widely used in fields such as chemical industry, food, medicine, agricultural, packing and environmental protection.
Compared with prior art, the present invention has following characteristics and beneficial effect:
(1) this is a raw material with natural Rhizoma amorphophalli glucomannan, by Rhizoma amorphophalli glucomannan is carried out physical and chemical modified, acquisition has thermoplastic konjak glucomannan acetate material, make it can use the processing of traditional thermoplastic working method, for the mass-producing development and application of Rhizoma amorphophalli glucomannan lays the foundation, create condition and the fine raw material resources is provided in the extensive application of aspects such as thermoplastic packing material, intermingling material for Rhizoma amorphophalli glucomannan, will in the biodegradable plastic in future, bring into play its due effect; This also can change the situation of China based on the outlet raw material, improve value-added content of product, and the aspect all has crucial meaning to adjusting the structure of rural undertaking, the reproducible konjaku resource of exploitation special product advantage, developing rural economy and new socialist countryside construction, increase farmers' income etc.;
(2) adopt the konjak glucomannan acetate thermoplastic material of the inventive method preparation to have good thermoplastic, can be used as thermoplastic packing material, intermingling material, mass-producing processing and production are carried out in available traditional extrusion molding, injection moulding, blow moiding method machine-shaping; Degrade fully and environmental friendliness after its goods use, can be widely used in fields such as chemical industry, food, medicine, agricultural, packing and environmental protection;
(3) adopt the present invention, preparation technology is simple, and environmental protection, cost are low, and operation is practical easily.
Description of drawings
Fig. 1 is differential scanning calorimeter (DSC) the analytic curve figure (annotate: heating rate is 10 ℃/min, nitrogen atmosphere) of Rhizoma amorphophalli glucomannan and konjak glucomannan acetate;
As can be seen from Figure 1, before decomposition temperature, glass transition does not appear in Rhizoma amorphophalli glucomannan, and a tangible glass transition has appearred in konjak glucomannan acetate; This explanation can be used method heating plasticizing moulding such as traditional extrusion molding, injection moulding through the konjak glucomannan acetate that obtains after the modification, has good thermoplastic.
Embodiment
Embodiment given below intends so that the invention will be further described; but can not be interpreted as it is limiting the scope of the invention; the person skilled in art to some nonessential improvement and adjustment that the present invention makes, still belongs to protection scope of the present invention according to the content of the invention described above.
The present invention is by in the following specific embodiment, and the umber of described each raw material is weight (for example kilogram) umber except that specified otherwise.
Embodiment 1:
A kind of preparation method of konjak glucomannan acetate thermoplastic material comprises:
It is that 25 ℃ of controlled temperature stir 1 hour after-filtration of swelling in 10% the Rhizoma amorphophalli glucomannan swelling control agent that 1 part of purifying Rhizoma amorphophalli glucomannan is added 50 parts of concentration; By weight the Rhizoma amorphophalli glucomannan after the swelling and 100 parts of dispersant were stirred 10 minutes, add 50 parts of acetic anhydride, 0.001 part of catalyzer, 30 ℃ of reactions of controlled temperature 0.1 hour; With reacted liquid cooling, Jia Shui, separate out white precipitate, filtration, washing, promptly got the cotton-shaped hydrophobicity konjak glucomannan acetate thermoplastic material of white loose in 5 hours in 30 ℃ of dryings.
Embodiment 2:
A kind of preparation method of konjak glucomannan acetate thermoplastic material comprises:
It is that 40 ℃ of controlled temperature stir 2 hours after-filtration of swelling in 20% the Rhizoma amorphophalli glucomannan swelling control agent that 5 parts of purifying Rhizoma amorphophalli glucomannans are added 100 parts of concentration; By weight the Rhizoma amorphophalli glucomannan after the swelling and 150 parts of dispersant were stirred 20 minutes, add 100 parts of acetic anhydride, 0.002 part of catalyzer, 45 ℃ of reactions of controlled temperature 1 hour; With reacted liquid cooling, Jia Shui, separate out white precipitate, filtration, washing, promptly got the cotton-shaped hydrophobicity konjak glucomannan acetate thermoplastic material of white loose in 10 hours in 45 ℃ of dryings.
Embodiment 3:
A kind of preparation method of konjak glucomannan acetate thermoplastic material comprises:
It is that 50 ℃ of controlled temperature stir 4 hours after-filtration of swelling in 40% the Rhizoma amorphophalli glucomannan swelling control agent that 10 parts of purifying Rhizoma amorphophalli glucomannans are added 150 parts of concentration; By weight the Rhizoma amorphophalli glucomannan after the swelling and 200 parts of dispersant were stirred 30 minutes, add 150 parts of acetic anhydride, 0.004 part of catalyzer, 60 ℃ of reactions of controlled temperature 2 hours; With reacted liquid cooling, Jia Shui, separate out white precipitate, filtration, washing, promptly got the cotton-shaped hydrophobicity konjak glucomannan acetate thermoplastic material of white loose in 15 hours in 60 ℃ of dryings.
Embodiment 4:
A kind of preparation method of konjak glucomannan acetate thermoplastic material comprises:
It is that 60 ℃ of controlled temperature stir 6 hours after-filtration of swelling in 60% the Rhizoma amorphophalli glucomannan swelling control agent that 15 parts of purifying Rhizoma amorphophalli glucomannans are added 200 parts of concentration; By weight the Rhizoma amorphophalli glucomannan after the swelling and 250 parts of dispersant were stirred 40 minutes, add 200 parts of acetic anhydride, 0.006 part of catalyzer, 75 ℃ of reactions of controlled temperature 3 hours; With reacted liquid cooling, Jia Shui, separate out white precipitate, filtration, washing, promptly got the cotton-shaped hydrophobicity konjak glucomannan acetate thermoplastic material of white loose in 20 hours in 70 ℃ of dryings.
Embodiment 5:
A kind of preparation method of konjak glucomannan acetate thermoplastic material comprises:
It is that 70 ℃ of controlled temperature stir 8 hours after-filtration of swelling in 70% the Rhizoma amorphophalli glucomannan swelling control agent that 20 parts of purifying Rhizoma amorphophalli glucomannans are added 250 parts of concentration; By weight the Rhizoma amorphophalli glucomannan after the swelling and 300 parts of dispersant were stirred 50 minutes, add 250 parts of acetic anhydride, 0.008 part of catalyzer, 85 ℃ of reactions of controlled temperature 4 hours; With reacted liquid cooling, Jia Shui, separate out white precipitate, filtration, washing, promptly got the cotton-shaped hydrophobicity konjak glucomannan acetate thermoplastic material of white loose in 25 hours in 80 ℃ of dryings.
Embodiment 6:
A kind of preparation method of konjak glucomannan acetate thermoplastic material comprises:
It is that 80 ℃ of controlled temperature stir 10 hours after-filtration of swelling in 80% the Rhizoma amorphophalli glucomannan swelling control agent that 30 parts of purifying Rhizoma amorphophalli glucomannans are added 300 parts of concentration; By weight the Rhizoma amorphophalli glucomannan after the swelling and 300 parts of dispersant were stirred 50 minutes, add 300 parts of acetic anhydride, 0.1 part of catalyzer, 95 ℃ of reactions of controlled temperature 5 hours; With reacted liquid cooling, Jia Shui, separate out white precipitate, filtration, washing, promptly got the cotton-shaped hydrophobicity konjak glucomannan acetate thermoplastic material of white loose in 30 hours in 90 ℃ of dryings.
Among the foregoing description 1-6: described purifying Rhizoma amorphophalli glucomannan is the konjac glucomanna that extracts from the plant konjaku, (can be again through ethanolic soln purify, median size be 1~100um), the weight percentage of konjac glucomanna 〉=50~80% wherein;
Among the foregoing description 1-6: a kind of in the water that described swelling control agent is methyl alcohol, ethanol or acetone (for the solvent) solution, described concentration is concentration of volume percent;
Among the foregoing description 1-6: described dispersion agent Glacial acetic acid; Described catalyzer is a methylsulphonic acid;
Embodiment 7:
A kind of preparation method of konjak glucomannan acetate thermoplastic material comprises the following steps:
A, Rhizoma amorphophalli glucomannan swelling: the purifying Rhizoma amorphophalli glucomannan of 1 weight part (unit kilogram, back with) is joined in the swelling control agent of 50 weight parts, under 25~80 ℃ temperature, stir 1 hour after-filtration of swelling, the swollen Rhizoma amorphophalli glucomannan;
Described purifying Rhizoma amorphophalli glucomannan is the konjac glucomanna that extracts from the plant konjaku, (can be again through ethanolic soln purify, median size be 1~100um), the weight percentage of konjac glucomanna 〉=50~80% wherein;
Described swelling control agent is that concentration of volume percent is a kind of in water (for the solvent) solution of 10% methyl alcohol, ethanol or acetone;
B, preparation konjak glucomannan acetate: the dispersant of swollen Rhizoma amorphophalli glucomannan and 100 weight parts was stirred 10 minutes, add the acetic anhydride of 50 weight parts, the catalyzer of 0.001 weight part again, reaction is 0.1 hour under 30~95 ℃ temperature, obtains the konjak glucomannan esters reacted solution;
Described dispersion agent is a Glacial acetic acid; Described catalyzer is a methylsulphonic acid;
C, with konjak glucomannan esters reacted solution cooling (to room temperature), add 3 times of described liquor capacities water, separate out (white) precipitation, filter, after the each water with 3 times of volumes of solids washs 3 times altogether, in 30~90 ℃ of dryings 5~30 hours, promptly make the cotton-shaped hydrophobic konjak glucomannan acetate thermoplastic material of white loose.
Embodiment 8:
A kind of preparation method of konjak glucomannan acetate thermoplastic material comprises the following steps:
A, Rhizoma amorphophalli glucomannan swelling: the purifying Rhizoma amorphophalli glucomannan of 30 weight parts (unit kilogram, back with) is joined in the swelling control agent of 300 weight parts, under 25~80 ℃ temperature, stir 10 hours after-filtration of swelling, the swollen Rhizoma amorphophalli glucomannan;
Described purifying Rhizoma amorphophalli glucomannan is the konjac glucomanna that extracts from the plant konjaku, (can be again through ethanolic soln purify, median size be 1~100um), the weight percentage of konjac glucomanna 〉=50~80% wherein;
Described swelling control agent is that concentration of volume percent is a kind of in water (for the solvent) solution of 80% methyl alcohol, ethanol or acetone;
B, preparation konjak glucomannan acetate: the dispersant of swollen Rhizoma amorphophalli glucomannan and 300 weight parts was stirred 50 minutes, add the acetic anhydride of 300 weight parts, the catalyzer of 0.1 weight part again, reaction is 5 hours under 30~95 ℃ temperature, obtains the konjak glucomannan esters reacted solution;
Described dispersion agent is a Glacial acetic acid; Described catalyzer is a methylsulphonic acid;
C, with konjak glucomannan esters reacted solution cooling (to room temperature), add 10 times of described liquor capacities water, separate out (white) precipitation, filter, after the each water with 10 times of volumes of solids washs 3 times altogether, in 30~90 ℃ of dryings 5~30 hours, promptly make the cotton-shaped hydrophobic konjak glucomannan acetate thermoplastic material of white loose.
Embodiment 9:
A kind of preparation method of konjak glucomannan acetate thermoplastic material comprises the following steps:
A, Rhizoma amorphophalli glucomannan swelling: the purifying Rhizoma amorphophalli glucomannan of 15 weight parts (unit kilogram, back with) is joined in the swelling control agent of 170 weight parts, under 25~80 ℃ temperature, stir 5 hours after-filtration of swelling, the swollen Rhizoma amorphophalli glucomannan;
Described purifying Rhizoma amorphophalli glucomannan is the konjac glucomanna that extracts from the plant konjaku, (can be again through ethanolic soln purify, median size be 1~100um), the weight percentage of konjac glucomanna 〉=50~80% wherein;
Described swelling control agent is that concentration of volume percent is a kind of in water (for the solvent) solution of 45% methyl alcohol, ethanol or acetone;
B, preparation konjak glucomannan acetate: the dispersant of swollen Rhizoma amorphophalli glucomannan and 200 weight parts was stirred 30 minutes, add the acetic anhydride of 160 weight parts, the catalyzer of 0.01 weight part again, reaction is 2.5 hours under 30~95 ℃ temperature, obtains the konjak glucomannan esters reacted solution;
Described dispersion agent is a Glacial acetic acid; Described catalyzer is a methylsulphonic acid;
C, with konjak glucomannan esters reacted solution cooling (to room temperature), add 5 times of described liquor capacities water, separate out (white) precipitation, filter, after the each water with 6 times of volumes of solids washs 2 times altogether, in 30~90 ℃ of dryings 5~30 hours, promptly make the cotton-shaped hydrophobic konjak glucomannan acetate thermoplastic material of white loose.
Embodiment 10-15:
A kind of preparation method of konjak glucomannan acetate thermoplastic material comprises the following steps:
A, Rhizoma amorphophalli glucomannan swelling: the purifying Rhizoma amorphophalli glucomannan is joined in the swelling control agent, under 25~80 ℃ temperature, stir 1~10 hour after-filtration of swelling, the swollen Rhizoma amorphophalli glucomannan;
Described purifying Rhizoma amorphophalli glucomannan is the konjac glucomanna that extracts from the plant konjaku, (can be again through ethanolic soln purify, median size be 1~100um), the weight percentage of konjac glucomanna 〉=50~80% wherein;
Described swelling control agent is that concentration of volume percent is a kind of in water (for the solvent) solution of 10~80% methyl alcohol, ethanol or acetone;
B, preparation konjak glucomannan acetate: swollen Rhizoma amorphophalli glucomannan and dispersant were stirred 10~50 minutes, add acetic anhydride, catalyzer again, under 30~95 ℃ temperature, reacted 0.1~5 hour, and obtained the konjak glucomannan esters reacted solution;
Described dispersion agent is a Glacial acetic acid; Described catalyzer is a methylsulphonic acid;
C, with konjak glucomannan esters reacted solution cooling (to room temperature), add 3~10 times of described liquor capacities water, separate out (white) precipitation, filter, after the each water with 3~10 times of volumes of solids washs 1-3 time altogether, in 30~90 ℃ of dryings 5~30 hours, promptly make the cotton-shaped hydrophobic konjak glucomannan acetate thermoplastic material of white loose.
The consumption of each feed composition (unit kilogram) weight part sees the following form:
Figure GSA00000107822600101
In the foregoing description: described dispersion agent can also replace with a kind of in acetone, the dimethyl sulfoxide (DMSO);
In the foregoing description: it is 98% the vitriol oil that described catalyzer can also replace with picoline, weight percentage, cross a kind of in the inorganic or organic acid such as chloric acid, methylsulfonic acid, methyl disulfonic acid, Witco 1298 Soft Acid or iron(ic) chloride.
The konjak glucomannan acetate thermoplastic material substitution value of the inventive method preparation is 0.5~3; water-intake rate is 1~8%; it is typical viscous-elastic material; its second-order transition temperature (Tg) is 120~200 ℃ (seeing accompanying drawing 1); has thermoplasticity preferably; can be used as thermoplastic packing material, intermingling material, mass-producing processing and production are carried out in available traditional extrusion molding, injection moulding, blow moiding method machine-shaping.Degrade fully and environmental friendliness after its goods use, can be widely used in fields such as chemical industry, food, medicine, agricultural, packing and environmental protection.
The invention is not restricted to the foregoing description, content of the present invention is described all can implement and have described good result.

Claims (3)

1. the preparation method of a konjak glucomannan acetate thermoplastic material is characterized in that comprising the following steps:
A, Rhizoma amorphophalli glucomannan swelling: the purifying Rhizoma amorphophalli glucomannan of 1~30 weight part is joined in the swelling control agent of 50~300 weight parts, under 25~80 ℃ temperature, stir 1~10 hour after-filtration of swelling, the swollen Rhizoma amorphophalli glucomannan;
Described purifying Rhizoma amorphophalli glucomannan is the konjac glucomanna that extracts from the plant konjaku, wherein the weight percentage 50~80% of konjac glucomanna;
Described swelling control agent is that concentration of volume percent is a kind of in the aqueous solution of 10~80% methyl alcohol, ethanol or acetone;
B, preparation konjak glucomannan acetate: the dispersant of swollen Rhizoma amorphophalli glucomannan and 100~300 weight parts was stirred 10~50 minutes, add the acetic anhydride of 50~300 weight parts, the catalyzer of 0.001~0.1 weight part again, under 30~95 ℃ temperature, reacted 0.1~5 hour, and obtained the konjak glucomannan esters reacted solution;
Described dispersion agent is a Glacial acetic acid;
Described catalyzer is a methylsulphonic acid;
C, with konjak glucomannan esters reacted solution cooling, add 3~10 times of described liquor capacities water, separate out precipitation, filter, after the each water with 3~10 times of volumes of solids washs 1-3 time altogether, in 30~90 ℃ of dryings 5~30 hours, promptly make konjak glucomannan acetate thermoplastic material.
2. by the preparation method of the described konjak glucomannan acetate thermoplastic material of claim 1, it is characterized in that: described dispersion agent replaces with a kind of in acetone, the dimethyl sulfoxide (DMSO).
3. by the preparation method of claim 1 or 2 described konjak glucomannan acetate thermoplastic materials, it is characterized in that: it is 98% the vitriol oil that described catalyzer replaces with picoline, weight percentage, cross a kind of in chloric acid, methylsulfonic acid, methyl disulfonic acid, Witco 1298 Soft Acid or the iron(ic) chloride.
CN 201010177363 2010-05-19 2010-05-19 Method for preparing konjak glucomannan acetate thermoplastic material Expired - Fee Related CN101831001B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201010177363 CN101831001B (en) 2010-05-19 2010-05-19 Method for preparing konjak glucomannan acetate thermoplastic material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201010177363 CN101831001B (en) 2010-05-19 2010-05-19 Method for preparing konjak glucomannan acetate thermoplastic material

Publications (2)

Publication Number Publication Date
CN101831001A CN101831001A (en) 2010-09-15
CN101831001B true CN101831001B (en) 2011-11-23

Family

ID=42715237

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201010177363 Expired - Fee Related CN101831001B (en) 2010-05-19 2010-05-19 Method for preparing konjak glucomannan acetate thermoplastic material

Country Status (1)

Country Link
CN (1) CN101831001B (en)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102899206B (en) * 2012-11-14 2014-07-09 西南科技大学 Preparation and use method of radionuclide decontaminant
CN104817647B (en) * 2015-04-30 2017-05-10 福建农林大学 Konjac glucomannan oven glove and production method thereof
CN105032366B (en) * 2015-07-10 2017-08-11 福建农林大学 A kind of konjaku glucomannan water body filter core and preparation method thereof
CN106633579B (en) * 2016-12-30 2019-03-05 四川生科力科技有限公司 The preparation method of thermoplasticity konjaku glucomannan nanocomposite

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1388158A (en) * 2002-06-10 2003-01-01 武汉大学 Biologically degradable packing film and its prepn
WO2005060937A1 (en) * 2003-12-23 2005-07-07 Chr. Hansen A/S Compressed tablets comprising viable probiotic microorganisms

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1388158A (en) * 2002-06-10 2003-01-01 武汉大学 Biologically degradable packing film and its prepn
WO2005060937A1 (en) * 2003-12-23 2005-07-07 Chr. Hansen A/S Compressed tablets comprising viable probiotic microorganisms

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
曾辉,钱和.高取代度水溶性高分子魔芋葡甘聚糖醋酸.《食品研究与开发》.2006,第27卷(第5期),49-53. *
肖丽霞1,王丽霞 ,陆蒸, 庞杰.魔芋葡甘聚糖的酯化及其产物特性.《无锡轻工大学学报》.2005,第24卷(第1期),34-37.
肖丽霞1,王丽霞,陆蒸, 庞杰.魔芋葡甘聚糖的酯化及其产物特性.《无锡轻工大学学报》.2005,第24卷(第1期),34-37. *

Also Published As

Publication number Publication date
CN101831001A (en) 2010-09-15

Similar Documents

Publication Publication Date Title
CN101497678B (en) Thermoplastic glucomannan and preparation thereof
CN102212212B (en) Method for preparing organosolv lignin modified starch thermoplastic composite material
CN113024897B (en) Preparation method of high-strength TPS starch for degradable material
CN101200393B (en) Membrane material for producing coated material and preparation technique thereof
CN100497478C (en) Method of preparing polylactic acid/silicon dioxide nano composite material from acidic silicasol
CN111690240A (en) Polylactic acid/nano cellulose composite material and preparation method thereof
CN108948690B (en) Polylactic acid-lignin-starch composite material and preparation method thereof
CN109853083B (en) Water-soluble degradable fiber and preparation method thereof
CN101831001B (en) Method for preparing konjak glucomannan acetate thermoplastic material
CN111349253B (en) Modified lignin/PBS (Poly Butylene succinate) bioplastic film and preparation method thereof
CN115124776B (en) Natural bamboo fiber modified PE or PP composite material and preparation method thereof
CN110129918B (en) Biomass-based composite material with high degradability for non-woven fabric and processing technology thereof
CN103012856A (en) Microcrystalline cellulose and polyvinyl alcohol reinforced starch-based full-biodegradable blending material and preparation method thereof
CN102250389B (en) Biodegradable polymer material compatibilized and blended by lignocellulose and preparation method thereof
CN106009570A (en) Method for preparing polylactic acid, bamboo nano-cellulose whisker and ultrafine bamboo charcoal composite material film
CN101831033A (en) Method for preparing environment-friendly modified carboxymethyl cellulose thermoplastic material
CN114874472A (en) Production method and application of biodegradable lignocellulose bioplastic
CN114292350A (en) Hemicellulose cinnamate, preparation method thereof and application thereof in biodegradable composite material
CN111234484B (en) Full-bio-based degradable polylactic acid/starch composite material and preparation method thereof
CN100506899C (en) Natural high molecular composite material and preparation method and application thereof
CN111518344A (en) Preparation method of low-temperature-resistant polyvinyl chloride composite material
CN114349881A (en) Preparation method of modified hemicellulose suitable for PBAT (poly (butylene adipate-co-terephthalate)) degradable membrane bag
CN114316537A (en) Biodegradable plastic and preparation method thereof
CN114437524A (en) Preparation method of sugarcane cellulose-based degradable composite material
Weng et al. A facile method of functional derivatization based on starch acetoacetate

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20111123

Termination date: 20130519