CN106800753A - A kind of preparation method of PBS bases environment-friendly materials - Google Patents
A kind of preparation method of PBS bases environment-friendly materials Download PDFInfo
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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
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H8/00—Macromolecular compounds derived from lignocellulosic materials
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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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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- 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
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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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
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Abstract
The present invention provides a kind of preparation method of PBS bases environment-friendly materials, comprises the following steps：(1) desert shell is crushed, water is boiled and obtains desert shell powder, desert shell powder is processed by steam explosion and obtains desert shell crude fibre；(2) the ultrasound soda boiling treatment of desert shell crude fibre soda boiling liquid is obtained into desert shell fiber；(3) hydroxyethyl cellulose and diethoxy phosphorous acyl chlorides are obtained into flame-proof modifier by graft reaction；(4) treatment is modified to desert shell fiber with flame-proof modifier and obtains modified desert shell fiber；(5) raw material is weighed；(6) raw material is mixed, extrusion obtains PBS base environment-friendly materials.The fire resistance of the PBS base environment-friendly materials that the present invention is prepared is stronger, and mechanical property is also preferable.
Description
Technical field
The present invention relates to field of polymer technology, more particularly to a kind of preparation method of PBS bases environment-friendly materials.
Background technology
Poly butylene succinate (hereinafter referred to as PBS) is synthesized into by succinic acid and butanediol through condensation polymerization, tree
Fat is creamy white, odorless tasteless, is easily decomposed by the enzyme in the multiple-microorganism or animal and plant body of nature, is metabolized, final to decompose
It is carbon dioxide and water, is typical fully biodegradable polymeric material.PBS has good biocompatibility and biology
Absorbability；Density 1.26g/cm3, 114 DEG C of fusing point, the difference of height and molecular weight distribution according to molecular weight, crystallinity exists
Between 30~45%.
PBS in the nineties in 20th century enter investigation of materials field, and rapidly become can wide popularization and application universal life
One of thing degradative plastics study hotspot material, heat resistance is good, and heat distortion temperature and product temperature in use can be more than 100 DEG C.
Its synthesis material source both can be petroleum resources, it is also possible to fermented by living resources and obtained, it may be said that PBS is biodegradable
Outstanding person in plastic material.
Publication No. CN103709688A, publication date are 2014.04.09, poly- U.S.'s biotechnology is limited to apply for artificial Anhui
The Chinese invention application documents of company disclose " PBS Wholly-degradable materials and its preparation method and application ", wherein, the PBS is complete
Degradable material contains PBS, PLA, filler and lubricant；On the basis of the gross weight of the material, the content of the PBS is
The content of 50-65 weight %, the PLA is 4-8 weight %, and the content of described filler is 30-40 weight % and the lubrication
The content of agent is 0.1-2 weight %.The invention had both maintained PBS former by adding bio-based degradable resin PLA in PBS
Some toughness enhances the modulus and rigidity of PBS again, while adding the fillers such as cheap starch, calcium carbonate, talcum powder ensureing
Both the modulus of PBS can have been improved on the basis of the original toughness of PBS, had increased rigidity, PBS degradable materials can be greatly lowered again
The price of material, so that the PBS materials can be used widely in injection, plastic uptake field.Though the PBS Wholly-degradable materials
The mechanical property of PBS is so improved, but it is still present inflammable defect as general PBS materials.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of PBS bases environment-friendly materials, the PBS bases prepared
The fire resistance of environment-friendly materials is stronger, and mechanical property is also preferable.
In order to solve the above technical problems, the technical scheme is that：
A kind of preparation method of PBS bases environment-friendly materials, comprises the following steps：
(1) added after desert shell is crushed with pulverizer in distilled water, 5h is incubated after being heated to 90 DEG C, drained after taking-up
Desert shell powder is obtained, is placed in and is processed 2min in micro-wave oven under 600W power, be transferred to after taking-up in the quick-fried device of sudden strain of a muscle, be passed through water vapour and add
2MPa is depressed into, moment pressure release after pressurize 2min, with 90 DEG C of hot water injection 10min after taking-up, obtains desert shell thick after drying
Fiber；
(2) NaOH, sodium tripolyphosphate, sodium metasilicate, hydrogen peroxide are added to the water, stirring is obtained to after being well mixed
Soda boiling liquid, soda boiling liquid is added by desert shell crude fibre, is placed in supersonic wave cleaning machine, and 3h is incubated after being heated to 90 DEG C, is taken out
After be washed to neutrality, at 90 DEG C drying obtain desert shell fiber；
(3) by hydroxyethyl cellulose addition chloroform, stirring adds reaction bulb to be placed in 60 DEG C to after being completely dissolved
Water-bath in, add triethylamine after be passed through nitrogen, will be added dropwise in reaction bulb in diethoxy phosphorous acyl chlorides 20min, stirring 24
Methanol extraction product will be added after hour, constant weight is dried under vacuum to 60 DEG C after ethanol filtration washing and is obtained flame-retardant modified
Agent；
(4) by flame-proof modifier addition chloroform, stirring adds desert shell fiber to after being well mixed, and is heated to
Stirring reaction 2 hours after 90 DEG C, are filtered after taking-up, and drying at 90 DEG C after filter cake chloroform cyclic washing is obtained into modified sand
Unconcerned shell fiber；
(5) raw material is weighed by following weight portion：100 parts of PBS, lubricant 1.5-2 parts, bulking agent 2-7 parts, antioxidant
0.3-0.8 parts, toughener 5-10 parts, 19-24 parts of the modified desert shell fiber that step (4) is obtained；
(6) raw material in addition to PBS is added into mixer, is stirred at 80 DEG C and add PBS, 110 DEG C to after being well mixed
Lower stirring to cooling and stirring machine is discharged to after well mixed, be cooled to after 60 DEG C of dischargings be transferred to vacuum exhaust formula exhaust outlet,
The double screw extruder of mouth mold, device for filtering impurities, melting extrusion obtains PBS base environment-friendly materials at 150-170 DEG C.
Preferably, in step (1) of the present invention, desert shell compares 1 with the weight of distilled water:18.
Preferably, in step (2) of the present invention, NaOH, sodium tripolyphosphate, sodium metasilicate, hydrogen peroxide, the weight of water
Amount is than being 6:5:5:3:500, desert shell fiber is 1 with the weight ratio of soda boiling liquid:18.
Preferably, in step (3) of the present invention, hydroxyethyl cellulose, triethylamine, diethoxy phosphorous acyl chlorides mole
Than being 1:1:1.8.
Preferably, in step (4) of the present invention, flame-proof modifier is 1 with the mass ratio of desert shell fiber:40.
Preferably, in step (4) of the present invention, the melt index of PBS is 5-10g/10min.
Preferably, in step (5) of the present invention, lubricant is the mixture of stearic acid and epoxidized soybean oil.
Preferably, in step (5) of the present invention, bulking agent is PBS-g-MAH.
Preferably, in step (5) of the present invention, antioxidant is antioxidant 1076.
Preferably, in step (5) of the present invention, toughener is PBAT.
Compared with prior art, the invention has the advantages that：
Fruit is a kind of dry fruit in desert, and with harder shell-desert shell, desert shell would generally be lost as food garbage
Abandon, desert shell contains the compositions such as cellulose, lignin, hemilignin, and the present invention is crushed after being collected, water is cooked off except table
Face impurity obtains desert shell powder, desert shell powder then is passed sequentially through into microwave treatment, steam explosion treatment, by desert shell
In cellulose and lignin, hemilignin efficiently separate and obtained desert shell crude fibre, it is then desert shell is slightly fine
Wesy's soda boiling liquid ultrasound soda boiling treatment, further eliminates lignin, hemicellulose and has obtained the preferable desert of mechanical property really
Case fibre, but desert shell fiber has inflammable defect, and compatibility therebetween and interface cohesion as PBS
Power is poor, so hydroxyethyl cellulose and diethoxy phosphorous acyl chlorides have been obtained fire resistance very by the present invention by graft reaction
Strong flame-proof modifier, is then modified treatment with flame-proof modifier to desert shell fiber, and desert shell fiber is introduced
The bound phosphate groups of hydrophobic aliphatic lateral chain and high flame retardant, effectively improve between desert shell fiber and PBS
Compatibility and interface binding power have obtained modified desert shell fiber, and PBS base environment-friendly materials greatly improved after being combined with PBS
Fire resistance and mechanical property.
Specific embodiment
Describe the present invention in detail below in conjunction with specific embodiment, herein illustrative examples of the invention and explanation
It is for explaining the present invention but not as a limitation of the invention.
Embodiment 1
PBS base environment-friendly materials are prepared in accordance with the following steps：
(1) added after desert shell is crushed with pulverizer in distilled water, desert shell compares 1 with the weight of distilled water:18,
5h is incubated after being heated to 90 DEG C, is drained after taking-up and is obtained desert shell powder, be placed in micro-wave oven and process 2min under 600W power, taken
It is transferred to after going out in the quick-fried device of sudden strain of a muscle, is passed through water vapour and is forced into 2MPa, moment pressure release after pressurize 2min is rushed after taking-up with 90 DEG C of hot water
10min is washed, desert shell crude fibre is obtained after drying；
(2) NaOH, sodium tripolyphosphate, sodium metasilicate, hydrogen peroxide are added to the water, NaOH, sodium tripolyphosphate,
Sodium metasilicate, hydrogen peroxide, the weight ratio of water are 6:5:5:3:500, stirring obtains soda boiling liquid to after being well mixed, by desert shell
Crude fibre adds soda boiling liquid, and desert shell fiber is 1 with the weight ratio of soda boiling liquid:18, it is placed in supersonic wave cleaning machine, it is heated to
3h is incubated after 90 DEG C, neutrality is washed to after taking-up, drying obtains desert shell fiber at 90 DEG C；
(3) by hydroxyethyl cellulose addition chloroform, stirring adds reaction bulb to be placed in 60 DEG C to after being completely dissolved
Water-bath in, add triethylamine after be passed through nitrogen, will be added dropwise in reaction bulb in diethoxy phosphorous acyl chlorides 20min, ethoxy
Cellulose, triethylamine, the mol ratio of diethoxy phosphorous acyl chlorides are 1:1:1.8, stirring will add methanol extraction anti-after 24 hours
Product is answered, being dried under vacuum to constant weight with 60 DEG C after ethanol filtration washing obtains flame-proof modifier；
(4) by flame-proof modifier addition chloroform, stirring adds desert shell fiber to after being well mixed, fire-retardant to change
Property agent and desert shell fiber mass ratio be 1:40, stirring reaction 2 hours after being heated to 90 DEG C are filtered, by filter cake after taking-up
Modified desert shell fiber is obtained with drying at 90 DEG C after chloroform cyclic washing；
(5) raw material is weighed by following weight portion：Melt index is 100 parts of the PBS of 5-10g/10min, stearic acid and epoxy
1.7 parts of the mixture of soybean oil, 3 parts of PBS-g-MAH, 0.3 part of antioxidant 1076,10 parts of PBAT, what step (4) was obtained changes
20 parts of property desert shell fiber；
(6) raw material in addition to PBS is added into mixer, is stirred at 80 DEG C and add PBS, 110 DEG C to after being well mixed
Lower stirring to cooling and stirring machine is discharged to after well mixed, be cooled to after 60 DEG C of dischargings be transferred to vacuum exhaust formula exhaust outlet,
The double screw extruder of mouth mold, device for filtering impurities, melting extrusion obtains PBS base environment-friendly materials at 150-170 DEG C.Embodiment 2
PBS base environment-friendly materials are prepared in accordance with the following steps：
(1) added after desert shell is crushed with pulverizer in distilled water, desert shell compares 1 with the weight of distilled water:18,
5h is incubated after being heated to 90 DEG C, is drained after taking-up and is obtained desert shell powder, be placed in micro-wave oven and process 2min under 600W power, taken
It is transferred to after going out in the quick-fried device of sudden strain of a muscle, is passed through water vapour and is forced into 2MPa, moment pressure release after pressurize 2min is rushed after taking-up with 90 DEG C of hot water
10min is washed, desert shell crude fibre is obtained after drying；
(2) NaOH, sodium tripolyphosphate, sodium metasilicate, hydrogen peroxide are added to the water, NaOH, sodium tripolyphosphate,
Sodium metasilicate, hydrogen peroxide, the weight ratio of water are 6:5:5:3:500, stirring obtains soda boiling liquid to after being well mixed, by desert shell
Crude fibre adds soda boiling liquid, and desert shell fiber is 1 with the weight ratio of soda boiling liquid:18, it is placed in supersonic wave cleaning machine, it is heated to
3h is incubated after 90 DEG C, neutrality is washed to after taking-up, drying obtains desert shell fiber at 90 DEG C；
(3) by hydroxyethyl cellulose addition chloroform, stirring adds reaction bulb to be placed in 60 DEG C to after being completely dissolved
Water-bath in, add triethylamine after be passed through nitrogen, will be added dropwise in reaction bulb in diethoxy phosphorous acyl chlorides 20min, ethoxy
Cellulose, triethylamine, the mol ratio of diethoxy phosphorous acyl chlorides are 1:1:1.8, stirring will add methanol extraction anti-after 24 hours
Product is answered, being dried under vacuum to constant weight with 60 DEG C after ethanol filtration washing obtains flame-proof modifier；
(4) by flame-proof modifier addition chloroform, stirring adds desert shell fiber to after being well mixed, fire-retardant to change
Property agent and desert shell fiber mass ratio be 1:40, stirring reaction 2 hours after being heated to 90 DEG C are filtered, by filter cake after taking-up
Modified desert shell fiber is obtained with drying at 90 DEG C after chloroform cyclic washing；
(5) raw material is weighed by following weight portion：Melt index is 100 parts of the PBS of 5-10g/10min, stearic acid and epoxy
1.5 parts of the mixture of soybean oil, 7 parts of PBS-g-MAH, 0.5 part of antioxidant 1076,8 parts of PBAT, it is modified that step (4) is obtained
18 parts of desert shell fiber；
(6) raw material in addition to PBS is added into mixer, is stirred at 80 DEG C and add PBS, 110 DEG C to after being well mixed
Lower stirring to cooling and stirring machine is discharged to after well mixed, be cooled to after 60 DEG C of dischargings be transferred to vacuum exhaust formula exhaust outlet,
The double screw extruder of mouth mold, device for filtering impurities, melting extrusion obtains PBS base environment-friendly materials at 150-170 DEG C.Embodiment 3
PBS base environment-friendly materials are prepared in accordance with the following steps：
(1) added after desert shell is crushed with pulverizer in distilled water, desert shell compares 1 with the weight of distilled water:18,
5h is incubated after being heated to 90 DEG C, is drained after taking-up and is obtained desert shell powder, be placed in micro-wave oven and process 2min under 600W power, taken
It is transferred to after going out in the quick-fried device of sudden strain of a muscle, is passed through water vapour and is forced into 2MPa, moment pressure release after pressurize 2min is rushed after taking-up with 90 DEG C of hot water
10min is washed, desert shell crude fibre is obtained after drying；
(2) NaOH, sodium tripolyphosphate, sodium metasilicate, hydrogen peroxide are added to the water, NaOH, sodium tripolyphosphate,
Sodium metasilicate, hydrogen peroxide, the weight ratio of water are 6:5:5:3:500, stirring obtains soda boiling liquid to after being well mixed, by desert shell
Crude fibre adds soda boiling liquid, and desert shell fiber is 1 with the weight ratio of soda boiling liquid:18, it is placed in supersonic wave cleaning machine, it is heated to
3h is incubated after 90 DEG C, neutrality is washed to after taking-up, drying obtains desert shell fiber at 90 DEG C；
(3) by hydroxyethyl cellulose addition chloroform, stirring adds reaction bulb to be placed in 60 DEG C to after being completely dissolved
Water-bath in, add triethylamine after be passed through nitrogen, will be added dropwise in reaction bulb in diethoxy phosphorous acyl chlorides 20min, ethoxy
Cellulose, triethylamine, the mol ratio of diethoxy phosphorous acyl chlorides are 1:1:1.8, stirring will add methanol extraction anti-after 24 hours
Product is answered, being dried under vacuum to constant weight with 60 DEG C after ethanol filtration washing obtains flame-proof modifier；
(4) by flame-proof modifier addition chloroform, stirring adds desert shell fiber to after being well mixed, fire-retardant to change
Property agent and desert shell fiber mass ratio be 1:40, stirring reaction 2 hours after being heated to 90 DEG C are filtered, by filter cake after taking-up
Modified desert shell fiber is obtained with drying at 90 DEG C after chloroform cyclic washing；
(5) raw material is weighed by following weight portion：Melt index is 100 parts of the PBS of 5-10g/10min, stearic acid and epoxy
1.9 parts of the mixture of soybean oil, 5 parts of PBS-g-MAH, 0.7 part of antioxidant 1076,6 parts of PBAT, it is modified that step (4) is obtained
19 parts of desert shell fiber；
(6) raw material in addition to PBS is added into mixer, is stirred at 80 DEG C and add PBS, 110 DEG C to after being well mixed
Lower stirring to cooling and stirring machine is discharged to after well mixed, be cooled to after 60 DEG C of dischargings be transferred to vacuum exhaust formula exhaust outlet,
The double screw extruder of mouth mold, device for filtering impurities, melting extrusion obtains PBS base environment-friendly materials at 150-170 DEG C.Embodiment 4
PBS base environment-friendly materials are prepared in accordance with the following steps：
(1) added after desert shell is crushed with pulverizer in distilled water, desert shell compares 1 with the weight of distilled water:18,
5h is incubated after being heated to 90 DEG C, is drained after taking-up and is obtained desert shell powder, be placed in micro-wave oven and process 2min under 600W power, taken
It is transferred to after going out in the quick-fried device of sudden strain of a muscle, is passed through water vapour and is forced into 2MPa, moment pressure release after pressurize 2min is rushed after taking-up with 90 DEG C of hot water
10min is washed, desert shell crude fibre is obtained after drying；
(2) NaOH, sodium tripolyphosphate, sodium metasilicate, hydrogen peroxide are added to the water, NaOH, sodium tripolyphosphate,
Sodium metasilicate, hydrogen peroxide, the weight ratio of water are 6:5:5:3:500, stirring obtains soda boiling liquid to after being well mixed, by desert shell
Crude fibre adds soda boiling liquid, and desert shell fiber is 1 with the weight ratio of soda boiling liquid:18, it is placed in supersonic wave cleaning machine, it is heated to
3h is incubated after 90 DEG C, neutrality is washed to after taking-up, drying obtains desert shell fiber at 90 DEG C；
(3) by hydroxyethyl cellulose addition chloroform, stirring adds reaction bulb to be placed in 60 DEG C to after being completely dissolved
Water-bath in, add triethylamine after be passed through nitrogen, will be added dropwise in reaction bulb in diethoxy phosphorous acyl chlorides 20min, ethoxy
Cellulose, triethylamine, the mol ratio of diethoxy phosphorous acyl chlorides are 1:1:1.8, stirring will add methanol extraction anti-after 24 hours
Product is answered, being dried under vacuum to constant weight with 60 DEG C after ethanol filtration washing obtains flame-proof modifier；
(4) by flame-proof modifier addition chloroform, stirring adds desert shell fiber to after being well mixed, fire-retardant to change
Property agent and desert shell fiber mass ratio be 1:40, stirring reaction 2 hours after being heated to 90 DEG C are filtered, by filter cake after taking-up
Modified desert shell fiber is obtained with drying at 90 DEG C after chloroform cyclic washing；
(5) raw material is weighed by following weight portion：Melt index is 100 parts of the PBS of 5-10g/10min, stearic acid and epoxy
1.8 parts of the mixture of soybean oil, 6 parts of PBS-g-MAH, 0.8 part of antioxidant 1076,5 parts of PBAT, it is modified that step (4) is obtained
23 parts of desert shell fiber；
(6) raw material in addition to PBS is added into mixer, is stirred at 80 DEG C and add PBS, 110 DEG C to after being well mixed
Lower stirring to cooling and stirring machine is discharged to after well mixed, be cooled to after 60 DEG C of dischargings be transferred to vacuum exhaust formula exhaust outlet,
The double screw extruder of mouth mold, device for filtering impurities, melting extrusion obtains PBS base environment-friendly materials at 150-170 DEG C.Embodiment 5
PBS base environment-friendly materials are prepared in accordance with the following steps：
(1) added after desert shell is crushed with pulverizer in distilled water, desert shell compares 1 with the weight of distilled water:18,
5h is incubated after being heated to 90 DEG C, is drained after taking-up and is obtained desert shell powder, be placed in micro-wave oven and process 2min under 600W power, taken
It is transferred to after going out in the quick-fried device of sudden strain of a muscle, is passed through water vapour and is forced into 2MPa, moment pressure release after pressurize 2min is rushed after taking-up with 90 DEG C of hot water
10min is washed, desert shell crude fibre is obtained after drying；
(2) NaOH, sodium tripolyphosphate, sodium metasilicate, hydrogen peroxide are added to the water, NaOH, sodium tripolyphosphate,
Sodium metasilicate, hydrogen peroxide, the weight ratio of water are 6:5:5:3:500, stirring obtains soda boiling liquid to after being well mixed, by desert shell
Crude fibre adds soda boiling liquid, and desert shell fiber is 1 with the weight ratio of soda boiling liquid:18, it is placed in supersonic wave cleaning machine, it is heated to
3h is incubated after 90 DEG C, neutrality is washed to after taking-up, drying obtains desert shell fiber at 90 DEG C；
(3) by hydroxyethyl cellulose addition chloroform, stirring adds reaction bulb to be placed in 60 DEG C to after being completely dissolved
Water-bath in, add triethylamine after be passed through nitrogen, will be added dropwise in reaction bulb in diethoxy phosphorous acyl chlorides 20min, ethoxy
Cellulose, triethylamine, the mol ratio of diethoxy phosphorous acyl chlorides are 1:1:1.8, stirring will add methanol extraction anti-after 24 hours
Product is answered, being dried under vacuum to constant weight with 60 DEG C after ethanol filtration washing obtains flame-proof modifier；
(4) by flame-proof modifier addition chloroform, stirring adds desert shell fiber to after being well mixed, fire-retardant to change
Property agent and desert shell fiber mass ratio be 1:40, stirring reaction 2 hours after being heated to 90 DEG C are filtered, by filter cake after taking-up
Modified desert shell fiber is obtained with drying at 90 DEG C after chloroform cyclic washing；
(5) raw material is weighed by following weight portion：Melt index is 100 parts of the PBS of 5-10g/10min, stearic acid and epoxy
1.6 parts of the mixture of soybean oil, 4 parts of PBS-g-MAH, 0.6 part of antioxidant 1076,7 parts of PBAT, it is modified that step (4) is obtained
24 parts of desert shell fiber；
(6) raw material in addition to PBS is added into mixer, is stirred at 80 DEG C and add PBS, 110 DEG C to after being well mixed
Lower stirring to cooling and stirring machine is discharged to after well mixed, be cooled to after 60 DEG C of dischargings be transferred to vacuum exhaust formula exhaust outlet,
The double screw extruder of mouth mold, device for filtering impurities, melting extrusion obtains PBS base environment-friendly materials at 150-170 DEG C.Embodiment 6
PBS base environment-friendly materials are prepared in accordance with the following steps：
(1) added after desert shell is crushed with pulverizer in distilled water, desert shell compares 1 with the weight of distilled water:18,
5h is incubated after being heated to 90 DEG C, is drained after taking-up and is obtained desert shell powder, be placed in micro-wave oven and process 2min under 600W power, taken
It is transferred to after going out in the quick-fried device of sudden strain of a muscle, is passed through water vapour and is forced into 2MPa, moment pressure release after pressurize 2min is rushed after taking-up with 90 DEG C of hot water
10min is washed, desert shell crude fibre is obtained after drying；
(2) NaOH, sodium tripolyphosphate, sodium metasilicate, hydrogen peroxide are added to the water, NaOH, sodium tripolyphosphate,
Sodium metasilicate, hydrogen peroxide, the weight ratio of water are 6:5:5:3:500, stirring obtains soda boiling liquid to after being well mixed, by desert shell
Crude fibre adds soda boiling liquid, and desert shell fiber is 1 with the weight ratio of soda boiling liquid:18, it is placed in supersonic wave cleaning machine, it is heated to
3h is incubated after 90 DEG C, neutrality is washed to after taking-up, drying obtains desert shell fiber at 90 DEG C；
(3) by hydroxyethyl cellulose addition chloroform, stirring adds reaction bulb to be placed in 60 DEG C to after being completely dissolved
Water-bath in, add triethylamine after be passed through nitrogen, will be added dropwise in reaction bulb in diethoxy phosphorous acyl chlorides 20min, ethoxy
Cellulose, triethylamine, the mol ratio of diethoxy phosphorous acyl chlorides are 1:1:1.8, stirring will add methanol extraction anti-after 24 hours
Product is answered, being dried under vacuum to constant weight with 60 DEG C after ethanol filtration washing obtains flame-proof modifier；
(4) by flame-proof modifier addition chloroform, stirring adds desert shell fiber to after being well mixed, fire-retardant to change
Property agent and desert shell fiber mass ratio be 1:40, stirring reaction 2 hours after being heated to 90 DEG C are filtered, by filter cake after taking-up
Modified desert shell fiber is obtained with drying at 90 DEG C after chloroform cyclic washing；
(5) raw material is weighed by following weight portion：Melt index is 100 parts of the PBS of 5-10g/10min, stearic acid and epoxy
1.7 parts of the mixture of soybean oil, 3 parts of PBS-g-MAH, 0.3 part of antioxidant 1076,10 parts of PBAT, what step (4) was obtained changes
20 parts of property desert shell fiber；
(6) raw material in addition to PBS is added into mixer, is stirred at 80 DEG C and add PBS, 110 DEG C to after being well mixed
Lower stirring to cooling and stirring machine is discharged to after well mixed, be cooled to after 60 DEG C of dischargings be transferred to vacuum exhaust formula exhaust outlet,
The double screw extruder of mouth mold, device for filtering impurities, melting extrusion obtains PBS base environment-friendly materials at 150-170 DEG C.
Fire resistance and mechanical property to PBS bases environment-friendly materials obtained in embodiment 1-6 and comparative example are carried out respectively
Test, comparative example is the Chinese invention application documents of Publication No. CN103709688A, and fire resistance is characterized by LOI values, LOI
Value is bigger, and proof fire resistance is stronger, and mechanical property aspect is characterized by tensile strength and bending strength, and tensile strength, bending are strong
Degree is bigger, and proof mechanical property is better.Test result see the table below：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative example | |
| LOI/% | 33 | 35 | 34 | 32 | 35 | 34 | 24 |
| Tensile strength/MPa | 27.1 | 27.3 | 27.2 | 26.8 | 27.0 | 26.7 | 26.3 |
| Bending strength/MPa | 32.6 | 32.8 | 32.4 | 32.5 | 32.9 | 32.7 | 34.3 |
As can be seen from the above table, the LOI values of the PBS base environment-friendly materials obtained by embodiment of the present invention 1-6 are significantly greater than
Comparative example, it was demonstrated that fire resistance is stronger, tensile strength is slightly larger than comparative example, and bending strength is then slightly below comparative example, it was demonstrated that mechanics
Better performances are suitable with comparative example.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
The personage for knowing this technology all can carry out modifications and changes under without prejudice to spirit and scope of the invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
Into all equivalent modifications or change, should be covered by claim of the invention.
Claims (10)
1. a kind of preparation method of PBS bases environment-friendly materials, it is characterised in that comprise the following steps：
(1) added after desert shell is crushed with pulverizer in distilled water, 5h is incubated after being heated to 90 DEG C, drained after taking-up and obtained
Desert shell powder, is placed in and processes 2min in micro-wave oven under 600W power, is transferred to after taking-up in the quick-fried device of sudden strain of a muscle, is passed through water vapour and is forced into
2MPa, moment pressure release after pressurize 2min, with 90 DEG C of hot water injection 10min after taking-up, obtains desert shell crude fibre after drying；
(2) NaOH, sodium tripolyphosphate, sodium metasilicate, hydrogen peroxide are added to the water, stirring obtains soda boiling to after being well mixed
Liquid, soda boiling liquid is added by desert shell crude fibre, is placed in supersonic wave cleaning machine, 3h is incubated after being heated to 90 DEG C, water after taking-up
Neutrality is washed till, drying obtains desert shell fiber at 90 DEG C；
(3) by hydroxyethyl cellulose addition chloroform, the water for adding reaction bulb to be placed in 60 DEG C is stirred to after being completely dissolved
In bath, nitrogen is passed through after adding triethylamine, will be added dropwise in reaction bulb in diethoxy phosphorous acyl chlorides 20min, stirred 24 hours
Methanol extraction product will be added afterwards, be dried under vacuum to constant weight with 60 DEG C after ethanol filtration washing and be obtained flame-proof modifier；
(4) by flame-proof modifier addition chloroform, stirring adds desert shell fiber to after being well mixed, and is heated to 90 DEG C
Stirring reaction 2 hours, are filtered after taking-up afterwards, and drying at 90 DEG C after filter cake chloroform cyclic washing is obtained into modified desert really
Case fibre；
(5) raw material is weighed by following weight portion：100 parts of PBS, lubricant 1.5-2 parts, bulking agent 2-7 parts, antioxidant 0.3-0.8
Part, toughener 5-10 parts, 19-24 parts of the modified desert shell fiber that step (4) is obtained；
(6) raw material in addition to PBS is added into mixer, is stirred at 80 DEG C and add PBS to after being well mixed, stirred at 110 DEG C
Mix to cooling and stirring machine is discharged to after well mixed, be cooled to after 60 DEG C of dischargings be transferred to vacuum exhaust formula exhaust outlet, mouth mold,
The double screw extruder of device for filtering impurities, melting extrusion obtains PBS base environment-friendly materials at 150-170 DEG C.
2. the preparation method of a kind of PBS bases environment-friendly materials according to claim 1, it is characterised in that：The step (1)
In, desert shell compares 1 with the weight of distilled water:18.
3. the preparation method of a kind of PBS bases environment-friendly materials according to claim 2, it is characterised in that：The step (2)
In, NaOH, sodium tripolyphosphate, sodium metasilicate, hydrogen peroxide, the weight ratio of water are 6:5:5:3:500, desert shell fiber with
The weight ratio of soda boiling liquid is 1:18.
4. the preparation method of a kind of PBS bases environment-friendly materials according to claim 3, it is characterised in that：The step (3)
In, hydroxyethyl cellulose, triethylamine, the mol ratio of diethoxy phosphorous acyl chlorides are 1:1:1.8.
5. the preparation method of a kind of PBS bases environment-friendly materials according to claim 4, it is characterised in that：The step (4)
In, flame-proof modifier is 1 with the mass ratio of desert shell fiber:40.
6. the preparation method of a kind of PBS bases environment-friendly materials according to claim 5, it is characterised in that：The step (4)
In, the melt index of PBS is 5-10g/10min.
7. the preparation method of a kind of PBS bases environment-friendly materials according to claim 6, it is characterised in that：The step (5)
In, lubricant is the mixture of stearic acid and epoxidized soybean oil.
8. the preparation method of a kind of PBS bases environment-friendly materials according to claim 7, it is characterised in that：The step (5)
In, bulking agent is PBS-g-MAH.
9. the preparation method of a kind of PBS bases environment-friendly materials according to claim 8, it is characterised in that：The step (5)
In, antioxidant is antioxidant 1076.
10. the preparation method of a kind of PBS bases environment-friendly materials according to claim 9, it is characterised in that：The step (5)
In, toughener is PBAT.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115141495A (en) * | 2022-07-25 | 2022-10-04 | 江苏中科睿赛污染控制工程有限公司 | Reinforced and toughened degradable material and preparation method thereof |
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| CN104047063A (en) * | 2014-06-25 | 2014-09-17 | 江南大学 | Method for preparing cotton stalk skin fiber for spinning with combination between steam explosion and alkali treatment |
| CN104448326A (en) * | 2014-11-23 | 2015-03-25 | 成都纺织高等专科学校 | Intumescent phosphorus-containing grafted polymer flame retardant as well as preparation and application thereof |
| CN104479385A (en) * | 2014-11-18 | 2015-04-01 | 江苏大学 | Preparation method of reinforced straw fiber composite material |
| CN105440602A (en) * | 2015-12-23 | 2016-03-30 | 山东国塑科技实业有限公司 | Coir/polybutylene succinate composite material and preparation method thereof |
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2016
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|---|---|---|---|---|
| CN104047063A (en) * | 2014-06-25 | 2014-09-17 | 江南大学 | Method for preparing cotton stalk skin fiber for spinning with combination between steam explosion and alkali treatment |
| CN104479385A (en) * | 2014-11-18 | 2015-04-01 | 江苏大学 | Preparation method of reinforced straw fiber composite material |
| CN104448326A (en) * | 2014-11-23 | 2015-03-25 | 成都纺织高等专科学校 | Intumescent phosphorus-containing grafted polymer flame retardant as well as preparation and application thereof |
| CN105440602A (en) * | 2015-12-23 | 2016-03-30 | 山东国塑科技实业有限公司 | Coir/polybutylene succinate composite material and preparation method thereof |
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| CN115141495A (en) * | 2022-07-25 | 2022-10-04 | 江苏中科睿赛污染控制工程有限公司 | Reinforced and toughened degradable material and preparation method thereof |
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