CN105602110B - A kind of preparation method of stearate hyperbranched polyether grafting sisal hemp crystallite - Google Patents
A kind of preparation method of stearate hyperbranched polyether grafting sisal hemp crystallite Download PDFInfo
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- CN105602110B CN105602110B CN201610063341.2A CN201610063341A CN105602110B CN 105602110 B CN105602110 B CN 105602110B CN 201610063341 A CN201610063341 A CN 201610063341A CN 105602110 B CN105602110 B CN 105602110B
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- 244000198134 Agave sisalana Species 0.000 title claims abstract description 42
- 235000011624 Agave sisalana Nutrition 0.000 title claims abstract description 42
- 239000004721 Polyphenylene oxide Substances 0.000 title claims abstract description 30
- 229920000570 polyether Polymers 0.000 title claims abstract description 30
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 239000000047 product Substances 0.000 claims abstract description 12
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 8
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- 239000008117 stearic acid Substances 0.000 claims abstract description 8
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 5
- BDAWXSQJJCIFIK-UHFFFAOYSA-N potassium methoxide Chemical compound [K+].[O-]C BDAWXSQJJCIFIK-UHFFFAOYSA-N 0.000 claims abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 238000010792 warming Methods 0.000 claims description 7
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000010992 reflux Methods 0.000 claims description 2
- 229920001587 Wood-plastic composite Polymers 0.000 abstract description 8
- 239000011155 wood-plastic composite Substances 0.000 abstract description 8
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 9
- 239000004743 Polypropylene Substances 0.000 description 8
- VXJPCEOTZNHHOA-UHFFFAOYSA-N [K].OC Chemical compound [K].OC VXJPCEOTZNHHOA-UHFFFAOYSA-N 0.000 description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000001746 injection moulding Methods 0.000 description 3
- 238000005453 pelletization Methods 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- -1 food-grade) Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 240000004246 Agave americana Species 0.000 description 1
- 235000008754 Agave americana Nutrition 0.000 description 1
- 244000099147 Ananas comosus Species 0.000 description 1
- 235000007119 Ananas comosus Nutrition 0.000 description 1
- 241001669679 Eleotris Species 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 238000012653 anionic ring-opening polymerization Methods 0.000 description 1
- 239000003519 biomedical and dental material Substances 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229940088417 precipitated calcium carbonate Drugs 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 102220040412 rs587778307 Human genes 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
- C08G65/332—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof
- C08G65/3322—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof acyclic
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Polyethers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of preparation method of stearate hyperbranched polyether grafting sisal hemp crystallite.Sisal hemp crystallite, tetrahydrofuran and potassium methoxide are weighed, is sequentially added in three-necked flask, N2Lower 1 h of temperature reaction of protection, adds dioxane and glycidol, after heat temperature raising reacts 24 ~ 26h, adds methanol and terminates reaction, pour into organic solvent and precipitate, filter, be dried in vacuo 24h, obtain superbrnaching end-hydroxy polyether grafting sisal hemp crystallite；Superbrnaching end-hydroxy polyether grafting sisal hemp crystallite, stearic acid and catalyst is weighed to add in three-necked flask in N2The lower heating stirring 11 ~ 13h of back flow reaction of protection, after reaction, product is poured into separation is precipitated in the beaker equipped with organic solvent, filtered, vacuum drying, that is, stearate hyperbranched polyether grafting sisal hemp crystallite is made.Abundant raw material of the present invention, cheap, environmental pollution is small, and preparation process is simple, and easy to large-scale production, made product being capable of effective toughening modifying wood plastic composite.
Description
Technical field
The invention belongs to field of high polymer material modification, is grafted more particularly to a kind of stearate hyperbranched polyether
The preparation method of sisal hemp crystallite.
Background technology
The appearance of PM2.5 indexs and increasingly severe haze weather have beaten alarm bell to our environmental protection.Make
The reason for into severe environmental pollution, is very much, but the still exhaust emission from enterprise, factory the most primary.Environmental protection
Key is to reduce the discharge of polluter, greatly develops ecological technique, this is to Resources for construction saving, friendly environment society's meaning
It is great.
In this context, wood plastic composite this advantages of can playing each component in material and fully profit
With discarded timber and plastics, reduce environmental pollution, the environment-friendly materials for reducing production cost are more and more subject to the extensive pass of people
Note.Wood plastic composite had not only had the formability of thermoplastic, but also had the secondary workability of similar wood, was widely used in
The fields such as packaging industry, railroad sleeper, building trade, garden courtyard and automobile inner decorative piece.Cellulose is that reserves are most abundant
Natural polymer, be inexhaustible natural reproducible resource.Sisal hemp also known as pineapple fibre, belong to American aloe
Section, is perennial leaf fibre crop, and a kind of hard fibre that world today's dosage is maximum, widest in area, its chemical composition
It is made of cellulose, lignin, three big component of hemicellulose and a small amount of extract.Since hard fibre characteristic has pure white, matter
Ground tough and tensile (pulling force is strong), springiness, sea water resistance leaching, rub resistance, be not easy cataclasm, and colloid is few, and the characteristic such as be not easy to skid, and is system
The high-quality raw material of standby wood plastic composite.
Dissaving polymer is a kind of novel high polymer material to grow up nearest decades, the three of its almost spherical shape
Dimension space molecular structure to tangle between strand it is less, thus with low viscosity, to be not easy crystallization and good fluidity etc. excellent
Physical and chemical performance more.Dissaving polymer can be synthesized by the method for " treating different things alike ", without carefully separation, operating process
Simply, preparation that can be extensive and inexpensive.Meanwhile this highly branched structure can be by chemical modification with a large amount of
Active function groups, there is important application in fields such as nano material, photoelectric material, bio-medical material and supramolecular materials
Value.
The present invention is proposed using glycidol and sisal hemp crystallite as raw material, and a kind of terminal hydroxy group is synthesized by anionic ring-opening polymerization
Hyperbranched polyether be grafted sisal hemp crystallite, then with stearic acid occur esterification be made stearate hyperbranched polyether grafting sisal hemp it is micro-
It is brilliant.This Research Thinking has no document report at present.
The content of the invention
The object of the present invention is to provide a kind of preparation method of stearate hyperbranched polyether grafting sisal hemp crystallite.
Concretely comprise the following steps：
(1) 0.16 ~ 0.32g sisal hemps crystallite, 10 ~ 20ml tetrahydrofurans and 40 ~ 80ul potassium methoxides are weighed, is sequentially added
In the three-necked flask of 250ml, N2Be warming up to 50 ~ 60 DEG C under protection, after 1 h of isothermal reaction, add 20 ~ 40ml dioxane and
1.8 ~ 4ml glycidols, after being heated to 92 ~ 95 DEG C of 24 ~ 26h of reaction, add 3 ~ 5ml methanol and terminate reaction, finally pour into
Precipitate, filter in 50ml organic solvents, be dried in vacuo 24h, superbrnaching end-hydroxy polyether grafting sisal hemp crystallite is made.
(2) raw material is weighed according to following mass ratio, superbrnaching end-hydroxy polyether grafting sisal hemp crystallite made from step (1):
Stearic acid:Catalyst=1:22~45:0.28 ~ 0.56, the raw material weighed is added in three-necked flask in N2In 120 ~ 130 under protection
11 ~ 13h of reaction is stirred at reflux at DEG C, after reaction, product is poured into precipitation point in the beaker equipped with 40 ~ 50ml organic solvents
From filtering, vacuum drying, products therefrom is stearate hyperbranched polyether grafting sisal hemp crystallite.
The organic solvent is one or both of ethanol and acetone.
The catalyst is the one or more in phosphoric acid, boric acid, p-methyl benzenesulfonic acid and sulfuric acid.
The method of the present invention has the following advantages：
(1) raw material resources are enriched, cheap, and environmental pollution is small.
(2) preparation process is simple, easy to large-scale production.
(3) stearate hyperbranched polyether grafting sisal hemp crystallite polarity obtained by is low with nonpolar acrylic resin
Intermiscibility is good, is remarkably improved interface compatibility, mechanical property and the processing rheological property of wood plastic composite.
Embodiment
Primary raw material used in following embodiments：Stearic acid（SA, 1801), sisal hemp crystallite（MCC, white powder）, shrink
Glycerine（GLD, analysis are pure）, methanol potassium solution (CH3OK, analysis are pure), tetrahydrofuran（Chemistry is pure）, dioxane（Chemistry is pure）,
Methanol（Chemistry is pure）, acetone（Chemistry is pure）, precipitated calcium carbonate（CaCO3, food-grade）, polypropylene (PP, T30S).
Embodiment 1：
(1) 0.16g sisal hemps crystallite, 15ml tetrahydrofurans and 40ul methanol potassium solutions are weighed, sequentially adds the three of 250ml
In mouth flask, N2It is warming up to 55 DEG C under protection, after 1 h of isothermal reaction, adds 20ml dioxane and 1.8ml glycidols,
After being heated to 95 DEG C of reaction 24h, add 3ml methanol and terminate reaction, finally pour into 50ml acetone and precipitate, filter, vacuum
Dry 24h, is made superbrnaching end-hydroxy polyether grafting sisal hemp crystallite.
(2) raw material is weighed according to following mass ratio, superbrnaching end-hydroxy polyether grafting sisal hemp crystallite made from step (1):
Stearic acid:P-methyl benzenesulfonic acid=1:22:0.28, the raw material weighed is added in three-necked flask in N2Stirred under protection at 130 DEG C
Back flow reaction 11h, after reaction, product is poured into separation is precipitated in the beaker equipped with 40ml acetone, filtered, vacuum drying,
Products therefrom is stearate hyperbranched polyether grafting sisal hemp crystallite.
Weigh 60g PP, 40g CaCO3, stearate hyperbranched polyether grafting sisal hemp crystallite made from 2g the present embodiment,
High-speed stirred mixes, and the extruding pelletization in double-screw plastic extrusion machine, is then injection moulded in vertical injection molding machine, up to sisal hemp
The CaCO that crystallite is modified3/ PP wood plastic composites.The heat decomposition temperature of the composite material is brought up to by unmodified 358 DEG C
474 DEG C, melt index brings up to 3.50g/10min by 1.71g/10min, and impact strength is by 19.1KJ/m2Bring up to 38.3KJ/
m2, toughness is by 112.5J/m3Bring up to 1255.8 J/m3。
Embodiment 2：
(1) 0.24g sisal hemps crystallite, 15ml tetrahydrofurans and 50ul methanol potassium solutions are weighed, sequentially adds the three of 250ml
In mouth flask, N2It is warming up to 55 DEG C under protection, after 1 h of isothermal reaction, adds 30ml dioxane and 3ml glycidols, add
After heat is warming up to 92 DEG C of reaction 26h, adds 3.5ml methanol and terminate reaction, finally pour into 50ml acetone and precipitate, filter, vacuum
Dry 24h, is made superbrnaching end-hydroxy polyether grafting sisal hemp crystallite.
(2) raw material is weighed according to following mass ratio, superbrnaching end-hydroxy polyether grafting sisal hemp crystallite made from step (1):
Stearic acid:P-methyl benzenesulfonic acid=1:30:0.38, the raw material weighed is added in three-necked flask in N2Stirred under protection at 125 DEG C
Back flow reaction 12h, after reaction, product is poured into separation is precipitated in the beaker equipped with 45ml acetone, filtered, vacuum drying,
Products therefrom is stearate hyperbranched polyether grafting sisal hemp crystallite.
Weigh 60g PP, 40g CaCO3, stearate hyperbranched polyether grafting sisal hemp crystallite made from 3g the present embodiment,
High-speed stirred mixes, and the extruding pelletization in double-screw plastic extrusion machine, is then injection moulded in vertical injection molding machine, up to sisal hemp
The CaCO that crystallite is modified3/ PP wood plastic composites.The heat decomposition temperature of the composite material is brought up to by unmodified 358 DEG C
476 DEG C, melt index brings up to 4.14g/10min by 1.71g/10min, and impact strength is by 19.1KJ/m2Bring up to 55.8KJ/
m2, toughness is by 112.5J/m3Bring up to 1750.1 J/m3。
Embodiment 3：
(1) 0.32g sisal hemps crystallite, 20ml tetrahydrofurans and 80ul methanol potassium solutions are weighed, sequentially adds the three of 250ml
In mouth flask, N2It is warming up to 55 DEG C under protection, after 1 h of isothermal reaction, adds 40ml dioxane and 4ml glycidols, add
After heat is warming up to 93.5 DEG C of reaction 25h, adds 4ml methanol and terminate reaction, finally pour into 50ml acetone and precipitate, filter, vacuum
Dry 24h, is made superbrnaching end-hydroxy polyether grafting sisal hemp crystallite.
(2) raw material is weighed according to following mass ratio, superbrnaching end-hydroxy polyether grafting sisal hemp crystallite made from step (1):
Stearic acid:P-methyl benzenesulfonic acid=1:45:0.56, the raw material weighed is added in three-necked flask in N2Stirred under protection at 120 DEG C
Back flow reaction 13h, after reaction, product is poured into separation is precipitated in the beaker equipped with 50ml acetone, filtered, vacuum drying,
Products therefrom is stearate hyperbranched polyether grafting sisal hemp crystallite.
Weigh 60g PP, 40g CaCO3, stearate hyperbranched polyether grafting sisal hemp crystallite made from 4g the present embodiment,
High-speed stirred mixes, and the extruding pelletization in double-screw plastic extrusion machine, is then injection moulded in vertical injection molding machine, up to sisal hemp
The CaCO that crystallite is modified3/ PP wood plastic composites.The heat decomposition temperature of the composite material is brought up to by unmodified 358 DEG C
477 DEG C, melt index brings up to 5.23g/10min by 1.71g/10min, and impact strength is by 19.1KJ/m2Bring up to 64.7KJ/
m2, toughness is by 112.5J/m3Bring up to 2186.7 J/m3。
Claims (1)
1. a kind of preparation method of stearate hyperbranched polyether grafting sisal hemp crystallite, it is characterised in that concretely comprise the following steps：
(1) 0.16 ~ 0.32g sisal hemps crystallite, 10 ~ 20mL tetrahydrofurans and 40 ~ 80 μ L potassium methoxides are weighed, sequentially add 250mL
Three-necked flask in, N2Be warming up to 50 ~ 60 DEG C under protection, after 1 h of isothermal reaction, add 20 ~ 40mL dioxane and 1.8 ~
4mL glycidols, after being heated to 92 ~ 95 DEG C of 24 ~ 26h of reaction, add 3 ~ 5mL methanol and terminate reaction, finally pour into 50mL
Precipitate, filter in organic solvent, be dried in vacuo 24h, superbrnaching end-hydroxy polyether grafting sisal hemp crystallite is made；
(2) raw material is weighed according to following mass ratio, superbrnaching end-hydroxy polyether grafting sisal hemp crystallite made from step (1):It is stearic
Acid:Catalyst=1:22~45:0.28 ~ 0.56, the raw material weighed is added in three-necked flask in N2Under protection at 120 ~ 130 DEG C
11 ~ 13h of reaction is stirred at reflux, after reaction, product is poured into separation is precipitated in the beaker equipped with 40 ~ 50mL organic solvents,
Filtering, vacuum drying, products therefrom are stearate hyperbranched polyether grafting sisal hemp crystallite；
The organic solvent is one or both of ethanol and acetone；
The catalyst is the one or more in phosphoric acid, boric acid, p-methyl benzenesulfonic acid and sulfuric acid.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554510A (en) * | 2013-11-02 | 2014-02-05 | 广西民族大学 | Amino-terminated modified cellulose, and preparation method and application thereof |
| CN103951830A (en) * | 2014-05-25 | 2014-07-30 | 桂林理工大学 | Preparation method of hyperbranched polyester graft modified sisal fiber cellulose microcrystal |
| CN104761749A (en) * | 2015-04-03 | 2015-07-08 | 四川大学 | Cellulose nanofiber hyperbranched modification method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008189732A (en) * | 2007-02-01 | 2008-08-21 | Fujifilm Corp | Cellulose acylate composition, cellulose acylate film, optical compensation sheet, polarizing plate and liquid crystal display |
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- 2016-01-31 CN CN201610063341.2A patent/CN105602110B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554510A (en) * | 2013-11-02 | 2014-02-05 | 广西民族大学 | Amino-terminated modified cellulose, and preparation method and application thereof |
| CN103951830A (en) * | 2014-05-25 | 2014-07-30 | 桂林理工大学 | Preparation method of hyperbranched polyester graft modified sisal fiber cellulose microcrystal |
| CN104761749A (en) * | 2015-04-03 | 2015-07-08 | 四川大学 | Cellulose nanofiber hyperbranched modification method |
Non-Patent Citations (1)
| Title |
|---|
| 超支化聚醚的合成与应用;黄萍珍 等;《高分子通报》;20101015(第10期);第97-105页 * |
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