CN107652448B - It is a kind of using carbon suboxide as the biomass micro mist surface modifying method of modifying agent - Google Patents
It is a kind of using carbon suboxide as the biomass micro mist surface modifying method of modifying agent Download PDFInfo
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- CN107652448B CN107652448B CN201711015587.3A CN201711015587A CN107652448B CN 107652448 B CN107652448 B CN 107652448B CN 201711015587 A CN201711015587 A CN 201711015587A CN 107652448 B CN107652448 B CN 107652448B
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Abstract
It is a kind of using carbon suboxide as the biomass micro mist surface modifying method of modifying agent, it is related to a kind of biomass micro mist surface modifying method；The present invention is by biomass micro mist, such as straw powder, powdered rice hulls, cotton stalk powder agricultural by-products, organic filler material as resins for universal use, prepare biosynthesis resin or wood plastic composite, it can turn waste into wealth, the cost of naval stores is reduced, saves petroleum resources, and can be improved the degradable ability of naval stores.However the main constituent of biomass micro mist is lignin and cellulose, contain a large amount of hydroxyl in its surface, it is on the whole in water-wet behavior, therefore poor with the binding ability of resin, it is easy to generate defect due to interface compatibility difference when naval stores squeezes out and forms, thus affects the comprehensive performance of product.
Description
Technical field
The present invention relates to a kind of biomass micro mist surface modifying methods.
Background technique
By biomass micro mist, such as straw powder, powdered rice hulls, cotton stalk powder agricultural by-products, organic as resins for universal use is filled out
Material is filled, biosynthesis resin or wood plastic composite is prepared, can turn waste into wealth, reduce the cost of naval stores, is saved
Petroleum resources, and can be improved the degradable ability of naval stores.However the main constituent of biomass micro mist is lignin
And a large amount of hydroxyl is contained on cellulose, surface, is on the whole water-wet behavior, therefore poor with the binding ability of resin, is easy
Defect is generated due to interface compatibility difference when naval stores squeezes out and forms, thus affects the comprehensive performance of product.
C3O2It can be seen as the acid anhydrides of malonic acid, thermally decomposed and be made by malonic acid.C3O2It is a kind of very active change
Object is closed, in addition to it addition reaction can occur with water, moreover it is possible to NH3, HCl, ROH (R is chain alkylene) etc. addition reaction occurs.C3O2's
Molecular structure is containing there are four cumulated double bonds, easily generation polymerization reaction.With C3O2Its reaction can be made full use of to live as modifying agent
Property and high osmosis as gas, reach good surface modification effect.
Summary of the invention
The present invention to solve the above-mentioned problems, and provides one kind with C3O2Table is carried out to biomass micro mist as modifying agent
The method of surface treatment.
Of the invention is a kind of using carbon suboxide as the biomass micro mist surface modifying method of modifying agent, it is to utilize biology
Matter micropowder processing device carries out what surface was modified, specifically follows the steps below:
One, malonic acid and phosphorus pentoxide are placed in pear-shaped flask first；And guarantee that the end of thermometer is located at pyriform
The bottom of flask；
Two, it is put into biomass micro mist to be processed in double-way pipe, while double-way pipe being placed in 80 DEG C in sink of the water surface
Under；Double-way pipe is connected to pear-shaped flask and air bag respectively；
Three, vacuum pump is connected to by valve, the air in reaction unit is discharged；Pear-shaped flask is heated using heating device
To 120~125 DEG C, after reacting 15~30min, stop heating, after pear-shaped flask is cooled to room temperature and air bag restores full size,
Take out biomass micro mist；It is modified by the biomass micro mist surface of modifying agent of carbon suboxide described in completing；
Wherein, phosphorus pentoxide and malonic acid are 2:1~2 according to molar ratio；Malonic acid and biomass micro mist to be processed
Mass ratio be 1:2~7；
The biomass micropowder processing device includes vavuum pump valve, pear-shaped flask, iron stand, heating device, bilateral
Pipe, sink, air bag and thermometer；
Through-hole on bottle stopper that vavuum pump valve passes through pear-shaped flask is connected with device, and thermometer is inserted into pyriform
The bottom of flask；The pear-shaped flask is fixed on iron stand by iron clamp, and heating device is provided with below pear-shaped flask；
It is placed in double-way pipe one end in sink and is connected with the through-hole being arranged in the top side of pear-shaped flask by rubber hose
Logical, the other end is connected to by rubber hose with the gas outlet of air bag.
C is prepared by the method for malonic acid and phosphorus pentoxide heat together3O2, pass through temperature and technology controlling and process C3O2Pressure,
Avoid it that polymerization reaction occurs.Utilize C3O2High reaction activity and high osmosis biomass micro mist is surface-treated, surface
C after processing3O2Chemical bonding is generated with the hydroxyl of biological surface, and formation color is micro- red on the surface of biomass, rich in double
The conjugated polycyclic diene structure of key (carbon-carbon double bond, C=O bond), as shown in Figure 7:
Compared with modified with existing surface, method provided by the invention is had the advantage that
First, through C3O2After surface treatment, although biological surface is still in water-wet behavior, chemical activity is significantly improved,
And the response characteristic with conjugated double bond, firm chemical bonding can be formed by addition reaction with resin matrix.
Second, main modifying agent is gas under the process conditions, therefore it can efficiently penetrate into porous biomass powder
In body, uniform and stable surface modification effect can achieve.
Third, main modifying agent is gas under the process conditions, and it is without the use of solvent, therefore can be modified to avoid surface
The agglomeration generated in the process by surface tension helps to improve the stability of technique and reaches better treatment effect.
Fourth, surface modifier reacts with the moisture in biomass micro mist, therefore can directly obtain after surface treatment
To the biomass micro mist of high dry.
Grafting rate using the modified biomass micro mist of method of the invention is 9.7%, iodine number 23.54.
It can be seen that by the SEM electromicroscopic photograph of biomass micro mist after handling through C3O2After processing, the shape on the surface of biomass
At the applicator similar to slurry, the surface for keeping biomass hydrophilic is partially clad.
Detailed description of the invention
Fig. 1 is the experimental provision schematic diagram of biomass micro mist of the present invention processing；Wherein, 1 is vavuum pump valve, and 2 be pyriform
Flask, 3 be iron stand, and 4 be alcolhol burner, and 5 be double-way pipe, and 6 be sink, and 7 be air bag, and 8 be thermometer；
Fig. 2 is the process units schematic diagram of biomass micro mist of the present invention processing；Wherein, 11 be reaction kettle, and 12 produce for reaction
Object discharge port, 13 be quick-opening device, and 14 be reaction kettle upper cover, and 15 be vacuum pump interface, and 16 be agitator motor, and 17 go out for gas
Mouthful, 18 be horizontal condenser, and 19 be pressure gauge, and 20 be storage device；
Fig. 3 is reaction kettle accompanying drawings；Wherein, 31 be bracket, and 32 be discharge port, and 33 be kettle under reaction vessel, and 34 are
Blender, 35 be kettle on reaction vessel, and 36 be injection port, and 37 be pressure gauge, and 38 be stirring motor；
Fig. 4 is the infrared absorpting light spectra of biomass micro mist；
Fig. 5 is C3O2The infrared absorpting light spectra of modified biomass micro mist；
Fig. 6 is C3O2The SEM photograph figure of modified biomass micro mist；
Fig. 7 is the conjugated polycyclic diene structure chart that double bond (carbon-carbon double bond, C=O bond) is rich on biological surface.
Specific embodiment
Specific embodiment 1: a kind of of present embodiment changes by the biomass micro mist surface of modifying agent of carbon suboxide
Property method, it is modified that it using biomass micropowder processing device carries out surface, specifically follow the steps below:
One, malonic acid and phosphorus pentoxide are placed in pear-shaped flask 2 first；And guarantee that the end of thermometer 8 is located at pears
The bottom of shape flask 2；
Two, it is put into biomass micro mist to be processed in double-way pipe 5, while double-way pipe 5 being placed in 80 DEG C in sink 6 of water
Under face；Double-way pipe 5 is connected to pear-shaped flask 2 and air bag 7 respectively；
Three, vacuum pump is connected to by valve 1, the air in reaction unit is discharged；Using heating device 4 by pear-shaped flask 2
120~125 DEG C are heated to, after reacting 15~30min, stops heating, is cooled to room temperature to pear-shaped flask 2 and air bag 7 restores former
After size, biomass micro mist is taken out；It is modified by the biomass micro mist surface of modifying agent of carbon suboxide described in completing；
Wherein, phosphorus pentoxide and malonic acid are 2:1~2 according to molar ratio；Malonic acid and biomass micro mist to be processed
Mass ratio be 1:2~7；
The biomass micropowder processing device include vavuum pump valve 1, pear-shaped flask 2, iron stand 3, heating device 4,
Double-way pipe 5, sink 6, air bag 7 and thermometer 8；
Through-hole on bottle stopper that vavuum pump valve 1 passes through pear-shaped flask 2 is connected with device, and thermometer 8 is inserted into
The bottom of pear-shaped flask 2；The pear-shaped flask 2 is fixed on iron stand 3 by iron clamp, is provided with below pear-shaped flask 2
Heating device 4；
5 one end of double-way pipe being placed in sink 6 passes through rubber hose with the through-hole being arranged in the top side of pear-shaped flask 2
Connection, the other end are connected to by rubber hose with the gas outlet of air bag 7.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: phosphorus pentoxide and malonic acid
It is 2:1 according to molar ratio.It is other same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first embodiment in that: phosphorus pentoxide and malonic acid
It is 2:1.5 according to molar ratio.It is other same as the specific embodiment one.
Specific embodiment 4: the present embodiment is different from the first embodiment in that: phosphorus pentoxide and malonic acid
It is 2:2 according to matter molar ratio.It is other same as the specific embodiment one.
Specific embodiment 5: the present embodiment is different from the first embodiment in that: malonic acid and life to be processed
The mass ratio of substance micro mist is 1:2~5.It is other same as the specific embodiment one.
Specific embodiment 6: the present embodiment is different from the first embodiment in that: heating device be alcolhol burner or
Person's regulating temperature electrothermal cover.It is other same as the specific embodiment one.
Specific embodiment 7: the present embodiment is different from the first embodiment in that: the biomass micro mist is
800 mesh~1600 mesh powdered rice hulls.It is other same as the specific embodiment one.
Specific embodiment 8: the present embodiment is different from the first embodiment in that: 120~125 DEG C are heated to, instead
Answer 20~30min.It is other same as the specific embodiment one.
Specific embodiment 9: the present embodiment is different from the first embodiment in that: it is to utilize biomass micro mist
Process units carries out what surface was modified, specifically follows the steps below:
One, malonic acid and phosphorus pentoxide are placed in reaction kettle 11, then reaction kettle 11 is vacuumized, make reaction kettle 11
In pressure be less than 1kPa；
Two, the coolant temperature of horizontal condenser 18 is adjusted to 0 DEG C；
Three, reaction kettle 11 is heated to 120 DEG C or more, the pressure controlled in reaction kettle 11 is less than 10kPa, by reaction product
It deposits in spare in storage device 20；
Four, the butadiene solution of biomass micro mist and benzoyl peroxide is added into reaction kettle 11, closes reaction kettle 11
And it vacuumizes；Reaction kettle 11 is heated to 80 DEG C；Under continuous agitation into reaction kettle 11 injection step three reaction
Product is cooled to room temperature after reacting 30min, and modified treated biomass micro mist is discharged in reacted product discharge port 12；Its
In, the pressure of reaction kettle 11 is controlled in injection process in 8~10kPa；
The molar ratio of the malonic acid and phosphorus pentoxide is 2:1~2；The mass ratio 1 of malonic acid and biomass micro mist:
2~7；
The biomass micro mist process units includes reaction kettle 11, agitator motor 16, horizontal condenser 18 and storage
Device 20；
Wherein, the gas vent of reaction kettle 11 is connected to the air inlet of horizontal condenser 18, the outlet of horizontal condenser 18
Mouth is connected to the air inlet of storage device 20；The agitator motor 16 is placed in 11 top of reaction kettle.
It is other same as the specific embodiment one.
Specific embodiment 10: the present embodiment is different from the first embodiment in that: it is to utilize biomass micro mist
Process units carries out what surface was modified, specifically follows the steps below:
One, malonic acid and phosphorus pentoxide are placed in reaction kettle 11, then reaction kettle 11 is vacuumized, make reaction kettle 11
In pressure be less than 1kPa；
Two, the coolant temperature of horizontal condenser 18 is adjusted to 0 DEG C；
Three, reaction kettle 11 is heated to 120 DEG C or more, the pressure controlled in reaction kettle 11 is less than 10kPa, by reaction product
It deposits in spare in storage device 20；
Four, biomass micro mist is added into reaction kettle 11, close reaction kettle 11 and vacuumizes；Reaction kettle 11 is heated to 70
℃；Into reaction kettle 11, the reaction product of injection step three is cooled to room temperature after reacting 20min under continuous agitation,
Modified treated biomass micro mist is discharged in reacted product discharge port 12；Wherein, reaction kettle 11 is controlled in injection process
Pressure in 1~5kPa；
The molar ratio of the malonic acid and phosphorus pentoxide is 2:1~2；The mass ratio 1 of malonic acid and biomass micro mist:
2~7；
The biomass micro mist process units includes reaction kettle 11, agitator motor 16, horizontal condenser 18 and storage
Device 20；
Wherein, the gas vent of reaction kettle 11 is connected to the air inlet of horizontal condenser 18, the outlet of horizontal condenser 18
Mouth is connected to the air inlet of storage device 20；The agitator motor 16 is placed in 11 top of reaction kettle.
It is other same as the specific embodiment one.
The content of present invention is not limited only to the content of the respective embodiments described above, the group of one of them or several specific embodiments
The purpose of invention also may be implemented in contract sample.
Beneficial effects of the present invention are verified by following embodiment:
Embodiment 1
Vavuum pump valve 1, pear-shaped flask 2, double-way pipe 5, gas conduit, thermometer 8, iron are assembled according to experimental provision Fig. 1
Pallet 3, sink 6 and air bag 7.Heating device can choose alcolhol burner or regulating temperature electrothermal cover, the air-tightness of check device.
0.02mol malonic acid is added in pear-shaped flask 2,0.03mol phosphorus pentoxide is added, is added in double-way pipe 5
Biomass micro mist (800 mesh powdered rice hulls) in 10g is to be processed connects experimental provision.Guarantee that pyriform burning is touched in the end of thermometer 8
The bottom of bottle 2.It heats and controls the temperature in pear-shaped flask 2 at 120~125 DEG C, malonic acid and phosphorus pentoxide occur at this time
Reaction generates C3O2Gas.The temperature for controlling sink 6 is 80 DEG C, works as C3O2Gas passes through 5 Shi Keyu biomass micro mist of double-way pipe
(powdered rice hulls) react, and reaction process is to C3O2Quickly, therefore the air pressure in air bag 7 is during the reaction always for gas consumption
State in safety.
It reacts and continues 20min, when the biomass micro mist in double-way pipe 5 is in blush, stop heating, it is cold to pear-shaped flask 2
But to room temperature, after air bag 7 restores original size, experimental rig is disassembled, the biomass micro mist that takes out that treated.This method is suitable for
Laboratory research uses.
The weight of precise reaction front and back biomass micro mist, the quality of biomass micro mist is increased to by 10g after reaction
10.87g, grafting rate 8.7%.
Fig. 4 and Fig. 5 is biomass micro mist respectively through C3O2The spectrogram of infrared absorption spectrum before and after modification.Due to life
Substance complicated component itself, and grafting amount is smaller, so C3O2Spectral shape before and after modification is more similar.C3O2It is modified
Treated biomass micro mist is in 1665.22cm-1And 1656.81cm-1There is obvious absorption peak at place, and it is double to respectively correspond carbon oxygen
The stretching vibration of key and carbon-carbon double bond, in spectrogram 1107.10cm-1There are small absorption peak, the flexible vibration of corresponding C-O-C key in place
It is dynamic, 1107.10cm-1The absorption peak at place is unobvious, it may be possible to because biomass powder itself is caused by existing stronger absorption at this.
Embodiment 2
100 parts of phosphorus pentoxides are added in reaction kettle 11 (see Fig. 2), 200 parts of malonic acid are added, closed reaction kettle 11 is fast
Opening apparatus.Together with vacuum pump, air in extraction kettle 11 makes the pressure in reaction kettle 11 be less than 1kPa.Condenser is set
18 coolant temperature is 0 DEG C.Agitator motor 16 is opened, reaction kettle 11 is heated to 120 DEG C or more, passes through heating power control
Pressure in reaction unit processed is less than 10kPa, to prevent product C3O2Autohemagglutination.Reaction product is converted into yellowish liquid through condensation
(in it is yellowish may be it is partially polymerized caused by), product is stored under conditions of 0 DEG C spare in holding vessel 20.
100 parts of biomass micro mist (800 mesh powdered rice hulls) are added (see Fig. 3) in reaction kettle 11, closed reaction kettle 11 is taken out true
It is empty.Reaction kettle 11 is heated to 70 DEG C, injects the C of liquid under conditions of lasting stirring into reaction kettle 11 by syringe pump3O2,
The pressure of reaction kettle 11 gradually rises in the process, by the injection volume of syringe pump control the pressure in reaction kettle 11 1~
5kPa, sustained response 20min stop injecting, after cooling down, modified place are discharged by the discharge port 12 of 11 bottom of reaction kettle
Biomass micro powder product after reason.
The content of double bond in the biomass micro mist after modification, C are measured with iodine number method3O2Biomass is micro- after modification
The iodine number of powder is 12.28, this explanation introduces a large amount of activated double bonds by modification on the surface of biomass.
The SEM electromicroscopic photograph of biomass micro mist is as shown in Figure 6 after processing.By electromicroscopic photograph it can be seen that through C3O2After processing,
The applicator similar to slurry is formd on the surface of biomass, the surface for keeping biomass hydrophilic is partially clad.
Embodiment 3
100 parts of phosphorus pentoxides are added in reaction kettle 11 (see Fig. 2), 200 parts of malonic acid are added, closed reaction kettle 11 is fast
Opening apparatus.Together with vacuum pump, air in extraction kettle 1 makes the pressure in reaction kettle 11 be less than 1kPa.Condenser 18 is set
Coolant temperature be 0 DEG C.Agitator motor 16 is opened, reaction kettle 11 is heated to 120 DEG C or more, is controlled by heating power
Pressure in reaction unit is less than 10kPa, to prevent product C3O2Autohemagglutination.Reaction product is converted into yellowish liquid through condensation
Yellowish may be partially polymerized caused), product is stored under conditions of 0 DEG C spare in holding vessel 10.
100 parts of biomass micro mist (800 mesh powdered rice hulls) are added (see Fig. 3) in reaction kettle 11, the fourth of benzoyl peroxide
1 part of diene solution (5%), closed reaction kettle 1 vacuumizes.Reaction kettle 11 is heated to 80 DEG C, is passed through under conditions of lasting stirring
Syringe pump injects the C of liquid into reaction kettle 113O2, the pressure of reaction kettle 11 gradually rises in the process, passes through syringe pump
Injection volume controls the pressure in reaction kettle 11 in 1~5kPa, sustained response 30min, stops injecting, after cooling down, by anti-
Answer the discharge port 12 of 11 bottom of kettle that modified treated biomass micro powder product is discharged.Use the modified biomass of this method
The grafting rate of micro mist is 9.7%, iodine number 23.54.
Claims (10)
1. a kind of using carbon suboxide as the biomass micro mist surface modifying method of modifying agent, it is characterised in that it is to utilize biology
Matter micropowder processing device carries out what surface was modified, specifically follows the steps below:
One, malonic acid and phosphorus pentoxide are placed in pear-shaped flask (2) first；And guarantee that the end of thermometer (8) is located at pears
The bottom of shape flask (2)；
Two, it is put into biomass micro mist to be processed in double-way pipe (5), while double-way pipe (5) is placed in sink (6) 80 DEG C
Underwater；Double-way pipe (5) is connected to pear-shaped flask (2) and air bag (7) respectively；
Three, vacuum pump is connected to by valve (1), the air in reaction unit is discharged；Using heating device (4) by pear-shaped flask
(2) it is heated to 120~125 DEG C, after reacting 15~30min, stops heating, be cooled to room temperature to pear-shaped flask (2) and air bag (7)
After restoring full size, biomass micro mist is taken out；It completes described using carbon suboxide as the biomass micro mist surface of modifying agent
It is modified；
Wherein, phosphorus pentoxide and malonic acid are 2:1~2 according to molar ratio；The matter of malonic acid and biomass micro mist to be processed
Amount is than being 1:2~7；
The biomass micropowder processing device includes vavuum pump valve (1), pear-shaped flask (2), iron stand (3), heating device
(4), double-way pipe (5), sink (6), air bag (7) and thermometer (8)；
Through-hole on bottle stopper that vavuum pump valve (1) passes through pear-shaped flask (2) is connected with device, and thermometer (8) is inserted into
To the bottom of pear-shaped flask (2)；The pear-shaped flask (2) is fixed on iron stand (3) by iron clamp, in pear-shaped flask (2)
Lower section is provided with heating device (4)；
It is soft by rubber with the through-hole that is arranged in the top side of pear-shaped flask (2) to be placed in double-way pipe (5) one end in sink (6)
Pipe connection, the other end are connected to by rubber hose with the gas outlet of air bag (7).
2. it is according to claim 1 a kind of using carbon suboxide as the biomass micro mist surface modifying method of modifying agent,
Be characterized in that phosphorus pentoxide and malonic acid according to molar ratio be 2:1.
3. it is according to claim 1 a kind of using carbon suboxide as the biomass micro mist surface modifying method of modifying agent,
Be characterized in that phosphorus pentoxide and malonic acid according to molar ratio be 2:1.5.
4. it is according to claim 1 a kind of using carbon suboxide as the biomass micro mist surface modifying method of modifying agent,
Be characterized in that phosphorus pentoxide and malonic acid according to matter molar ratio be 2:2.
5. it is according to claim 1 a kind of using carbon suboxide as the biomass micro mist surface modifying method of modifying agent,
The mass ratio for being characterized in that malonic acid and biomass micro mist to be processed is 1:2~5.
6. it is according to claim 1 a kind of using carbon suboxide as the biomass micro mist surface modifying method of modifying agent,
It is characterized in that heating device is alcolhol burner or regulating temperature electrothermal cover.
7. it is according to claim 1 a kind of using carbon suboxide as the biomass micro mist surface modifying method of modifying agent,
It is characterized in that the biomass micro mist is 800 mesh~1600 mesh powdered rice hulls.
8. it is according to claim 1 a kind of using carbon suboxide as the biomass micro mist surface modifying method of modifying agent,
It is characterized in that being heated to 120~125 DEG C, reacts 20~30min.
9. a kind of using carbon suboxide as the biomass micro mist surface modifying method of modifying agent, it is characterised in that it is to utilize biology
Matter micro mist process units carries out what surface was modified, specifically follows the steps below:
One, malonic acid and phosphorus pentoxide are placed in reaction kettle (11), then reaction kettle (11) is vacuumized, makes reaction kettle
(11) pressure in is less than 1kPa；
Two, the coolant temperature of horizontal condenser (18) is adjusted to 0 DEG C；
Three, reaction kettle (11) is heated to 120 DEG C or more, the pressure in control reaction kettle (11) is less than 10kPa, by reaction product
It deposits in spare in storage device (20)；
Four, the butadiene solution of biomass micro mist and benzoyl peroxide is added into reaction kettle (11), closes reaction kettle (11)
And it vacuumizes；Reaction kettle (11) is heated to 80 DEG C；The injection step three in reaction kettle (11) under continuous agitation
Reaction product is cooled to room temperature after reacting 30min, treated biomass that the discharge of reacted product discharge port (12) is modified
Micro mist；Wherein, the pressure of reaction kettle (11) is controlled in injection process in 8~10kPa；
The molar ratio of the malonic acid and phosphorus pentoxide is 2:1~2；The mass ratio of malonic acid and biomass micro mist is 1:2
~7；
The biomass micro mist process units includes reaction kettle (11), agitator motor (16), horizontal condenser (18) and storage
Cryopreservation device (20)；
Wherein, the gas vent of reaction kettle (11) is connected to the air inlet of horizontal condenser (18), and horizontal condenser (18) goes out
Port is connected to the air inlet of storage device (20)；The agitator motor (16) is placed in above reaction kettle (11).
10. a kind of using carbon suboxide as the biomass micro mist surface modifying method of modifying agent, it is characterised in that it is to utilize life
Substance micro mist process units carries out what surface was modified, specifically follows the steps below:
One, malonic acid and phosphorus pentoxide are placed in reaction kettle (11), then reaction kettle (11) is vacuumized, makes reaction kettle
(11) pressure in is less than 1kPa；
Two, the coolant temperature of horizontal condenser (18) is adjusted to 0 DEG C；
Three, reaction kettle (11) is heated to 120 DEG C or more, the pressure in control reaction kettle (11) is less than 10kPa, by reaction product
It deposits in spare in storage device (20)；
Four, biomass micro mist is added into reaction kettle (11), close reaction kettle (11) and vacuumizes；Reaction kettle (11) is heated to
70℃；The reaction product of injection step three is cooled to after reacting 20min in reaction kettle (11) under continuous agitation
Room temperature, the discharge of reacted product discharge port (12) is modified treated biomass micro mist；Wherein, it is controlled in injection process anti-
Answer the pressure of kettle (11) in 1~5kPa；
The molar ratio of the malonic acid and phosphorus pentoxide is 2:1~2；The mass ratio of malonic acid and biomass micro mist is 1:2
~7；
The biomass micro mist process units includes reaction kettle (11), agitator motor (16), horizontal condenser (18) and storage
Cryopreservation device (20)；
Wherein, the gas vent of reaction kettle (11) is connected to the air inlet of horizontal condenser (18), and horizontal condenser (18) goes out
Port is connected to the air inlet of storage device (20)；The agitator motor (16) is placed in above reaction kettle (11).
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| JP2004035814A (en) * | 2002-07-05 | 2004-02-05 | Toray Ind Inc | Method of producing cellulose ester composition |
| CN1470532A (en) * | 2003-06-12 | 2004-01-28 | 中国科学院广州化学研究所 | Surface modifier of ultrafin and nano mcirocrystal cellulose |
| CN102459349A (en) * | 2009-04-15 | 2012-05-16 | 伊士曼化工公司 | Regioselectively substituted cellulose esters produced in a tetraalkylammonium alkylphosphate ionic liquid process and products produced therefrom |
| CN103502321A (en) * | 2011-05-25 | 2014-01-08 | 英派尔科技开发有限公司 | Treating lignocellulosic materials |
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