CN108465455A - A kind of novel environment-friendly composite material and its preparation process - Google Patents
A kind of novel environment-friendly composite material and its preparation process Download PDFInfo
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- CN108465455A CN108465455A CN201810339095.8A CN201810339095A CN108465455A CN 108465455 A CN108465455 A CN 108465455A CN 201810339095 A CN201810339095 A CN 201810339095A CN 108465455 A CN108465455 A CN 108465455A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/025—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with wetted adsorbents; Chromatography
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- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0218—Compounds of Cr, Mo, W
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0288—Halides of compounds other than those provided for in B01J20/046
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2257/00—Components to be removed
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- B01D2257/502—Carbon monoxide
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Abstract
The invention discloses a kind of novel environment-friendly composite material and its preparation process, the novel environment-friendly composite material, each raw material weight percentage is：Chromium trichloride 5 8%, tungsten hexachloride 5 8%, molybdenum pentachloride 8 12%, alumine hydroxide colloid 10 15%, modified galapectite 60 80%；It is inserted into modified galapectite interlayer by alumine hydroxide colloid particle fusion and obtains composite porous material, increase the absorption property of galapectite, chromium trichloride, the composite porous material adsorption reaction of tungsten hexachloride and molybdenum pentachloride and preparation obtains novel environment-friendly composite material, intelligent control carbon monoxide absorbing reaction kettle, CO gas in reaction dissolvent respectively with the chromium on environment-friendly composite material, tungsten, molybdenum carries out ligand complex, chromium, wolfram element, molybdenum element can be coordinated with 6 carbon monoxide, substantially increase adsorption reaction performance of the novel environment-friendly composite material to carbon monoxide, energy conservation and environmental protection.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of novel environment-friendly composite material and its preparation process.
Background technology
In the industrial production, it is generated in fuel combustion process and largely contains dust flue gas, dust flue gas is gas and flue dust
Mixture, be pollution residential block air the main reason for.The ingredient of flue gas is very complicated, and gas includes water vapour, titanium dioxide
Sulphur, nitrogen, oxygen, carbon monoxide and carbon dioxide etc., if being directly discharged into the pollution that can be caused in air to environment.In flue gas
If carbon monoxide detach not in time, serious problem of environmental pollution can be caused by being discharged into air, at the same human body sucking after
It can be poisoned, in addition carbon monoxide is objectionable impurities in some industrial gasses, can make catalyst poisoning.It is fast with industrial economy
Speed development increasingly emphasizes energy-saving and emission-reduction and country to the limitation and requirement of pollutant emission and carbon monoxide in work in production
Importance in industry production, develops energy-efficient adsorption separation technology, to meet in industrial products containing carbon monoxide and tail gas
Separation, purification and the purification of each substance, there is important social and economic implications.
Invention content
The purpose of the present invention is to provide a kind of novel environment-friendly composite material and its preparation processes, solve carbon monoxide gas
The problem of body exhaust emission.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of novel environment-friendly composite material, each raw material weight percentage are：It is chromium trichloride 5-8%, tungsten hexachloride 5-8%, phosphoric
Molybdenum 8-12%, alumine hydroxide colloid 10-15%, modified galapectite 60-80%.
Further, the preparation method of the modification galapectite is：Galapectite is added in ball mill and is ground, is added
Water is modulated into the galapectite solution of a concentration of 30-35%, and the concentrated sulfuric acid solution of 45-50% is added while stirring, waits for clayish solution
When pH is 2.3-3.0, stop the addition of the concentrated sulfuric acid, continue to stir 10-15min, the pH for measuring galapectite solution again is 2.0-
When 2.5, the clayish solution of acidification is put into water bath sonicator instrument, in the case where bath temperature is 60-70 DEG C, ultrasonic 10min, in 60-
Heat preservation takes out supernatant after standing at 70 DEG C, and purifying galapectite is obtained by filtration, and stops when using purifying water washing to pH for 6.5-7.0
It only washs, the purifying galapectite after washing is put into vacuum drying chamber, be -0.01-0.06MPa, temperature 62- in vacuum degree
Dry 24-30h at 66 DEG C when the moisture of galapectite to be purified≤12%, takes out dry purifying galapectite and is put into Muffle furnace,
3-5h is calcined at 900-1000 DEG C, 325 mesh is crushed and sieves up to the modification galapectite activated.
A kind of preparation process of novel environment-friendly composite material, specifically includes following steps：
S1, by alumine hydroxide colloid be put into spray drying bed granulation is dried；
S2, alumine hydroxide colloid particle and modified galapectite are put into screw extruder progress melting extrusion, obtained compound porous
Material；
S3, chromium trichloride, tungsten hexachloride and molybdenum pentachloride are added in reactor, under the protection of n-hexane, S2 systems is added
Standby composite porous material is stirred at reflux adsorption reaction 6-8h, filtering, is obtained after 40-50h is dried in vacuo at 55-60 DEG C
Novel environment-friendly composite material.
Further, one area's temperature of screw extruder described in step S2 is 120-130 DEG C, and two area's temperature of screw extruder is
300-315℃。
Further, the novel environment-friendly composite material that step S3 is obtained is applied to carry out an oxygen in carbon monoxide absorbing reaction kettle
Change the absorption of carbon.
Further, the carbon monoxide absorbing reaction kettle includes reaction kettle, material cores, solvent tank, air inlet pipe and outlet
The upper end of pipe, reaction kettle is connected with air inlet pipe and an air outlet pipe respectively, and air inlet pipe is symmetrically connected to the upper end both sides of reaction kettle, outlet
Pipe is connected to the upper end middle of reaction kettle, and lower end and the solvent tank of reaction kettle are connected, and material cores are mounted on the inside of reaction kettle；
It is connected with heater strip on the reaction kettle inner wall, reactor bottom is connected with temperature sense meter, on temperature sense meter
Temperature probe gos deep between material cores；
The material cores are interference fitted with reaction kettle inner wall, and the shapes of material cores is circular comb shape, and material cores are by described novel
Environment-friendly composite material is made；
Reaction dissolvent is contained in the solvent tank, solvent pot bottom is connected with solvent pipe, the bottom of solvent pipe and reaction kettle
Portion connects, and pump and the first solenoid valve are connected in solvent pipe；
The air inlet pipe passes through the bottom of material cores intercalation reaction kettle, air inlet pipe to be interference fitted with material cores, the bottom of air inlet pipe
End is equipped with Conic nozzle；
The escape pipe is equipped with four-way interface, and the first branch pipe, the second branch pipe and third branch pipe are connected on four-way interface, the
Carbonmonoxide detector is connected on one branch pipe, carbonmonoxide detector is used to detect the carbon monoxide content in escape pipe, the
One end of two branch pipes is connected to air inlet pipe, and second solenoid valve is connected on the second branch pipe, third electromagnetism is connected on third branch pipe
Valve；
Temperature sense meter, pump, the first solenoid valve, carbonmonoxide detector, second solenoid valve and the third solenoid valve is logical
Cordless communication network is crossed to connect with central controller.
Further, the reaction dissolvent is n,N-Dimethylformamide or dimethyl sulfoxide (DMSO).
Further, the working method of the carbon monoxide absorbing reaction kettle is：Central controller controls open pump and the
One solenoid valve, reaction dissolvent is passed through in reaction kettle, after the liquid level of reaction dissolvent floods material cores completely, closes pump and first
Solenoid valve is opened heater strip and is heated, kept the temperature when the temperature of temperature sense meter is 110-130 DEG C, be passed through carbon monoxide gas
Body opens third solenoid valve, and the content of carbon monoxide in an outlet gas is detected every 10min carbonmonoxide detectors,
When carbon monoxide content exceeds setting value, stops CO gas and be passed through, close third solenoid valve, open the second electromagnetism
Valve, while pump and the first solenoid valve withdrawal reaction dissolvent are opened, replace material cores.
Beneficial effects of the present invention：
A kind of novel environment-friendly composite material provided by the invention and its preparation process, are inserted by alumine hydroxide colloid particle fusion
Modified galapectite interlayer obtains composite porous material, increases the absorption property of galapectite, chromium trichloride, tungsten hexachloride and pentachloro-
The composite porous material adsorption reaction for changing molybdenum and preparation obtains novel environment-friendly composite material, intelligent control carbon monoxide absorbing reaction
Kettle, CO gas in reaction dissolvent respectively on environment-friendly composite material chromium, tungsten, molybdenum carry out ligand complex, chromium,
Wolfram element, molybdenum element can be coordinated with 6 carbon monoxide, substantially increase novel environment-friendly composite material to carbon monoxide
Adsorption reaction performance, energy conservation and environmental protection.
Certainly, it implements any of the products of the present invention and does not necessarily require achieving all the advantages described above at the same time.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, will be described below to embodiment required
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is carbon monoxide absorbing reaction process flow chart of the present invention；
1- reaction kettles, 11- heater strips, 12- temperature sense meters, 121- temperature probes；2- material cores；3- solvent tanks, 31- solvents
Pipe, 32- pumps, the first solenoid valves of 33-；4- air inlet pipe, 41- nozzles；5- escape pipes, 51- four-way interfaces, the first branch pipes of 52-, 53-
Second branch pipe, 54- third branch pipes, 55- carbonmonoxide detectors, 56- second solenoid valves, 57- third solenoid valves.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained all other without creative efforts
Embodiment shall fall within the protection scope of the present invention.
The present invention is a kind of novel environment-friendly composite material, and each raw material weight is：Chromium trichloride 6g, tungsten hexachloride 6g, pentachloro-
Change molybdenum 10g, alumine hydroxide colloid 12g, modified galapectite 66g；
The preparation method of the modification galapectite is：
Galapectite is added in ball mill and is ground, water is added to be modulated into a concentration of 33% galapectite solution, is added while stirring
The concentrated sulfuric acid solution for entering 48% stops the addition of the concentrated sulfuric acid when pH for measuring clayish solution is 2.6, continues to stir 12min, again
The pH for measuring galapectite solution is 2.6, and the clayish solution of acidification is put into water bath sonicator instrument, in the case where bath temperature is 66 DEG C,
Ultrasonic 10min takes out supernatant after heat preservation standing at 65 DEG C, purifying galapectite is obtained by filtration, using purifying water washing to pH
It is 6.8, stops washing, the purifying galapectite after washing is put into vacuum drying chamber, is -0.01MPa in vacuum degree, temperature is
Dry 25h at 65 DEG C, the moisture for measuring purifying galapectite is 10%, takes out dry purifying galapectite and is put into Muffle furnace,
4h is calcined at 920 DEG C, 325 mesh is crushed and sieves up to the modification galapectite activated；
A kind of preparation process of novel environment-friendly composite material, specifically includes following steps：
S1, by alumine hydroxide colloid be put into spray drying bed granulation is dried；
S2, alumine hydroxide colloid particle and modified galapectite are put into screw extruder progress melting extrusion, screw extruder one
Area's temperature is 125 DEG C, and two area's temperature of screw extruder is 308 DEG C, and alumine hydroxide colloid particle fusion is inserted into modified galapectite layer
Between obtain composite porous material, increase the absorption property of galapectite；
S3, chromium trichloride, tungsten hexachloride and molybdenum pentachloride are added in reactor, under the protection of n-hexane, S2 systems is added
Standby composite porous material is stirred at reflux adsorption reaction 7h, filtering, and novel environment friendly is obtained after 42h is dried in vacuo at 56 DEG C
Composite material.
Refering to Figure 1, the novel environment-friendly composite material is applied to carry out one in carbon monoxide absorbing reaction kettle
The absorption of carbonoxide, the carbon monoxide absorbing reaction kettle include reaction kettle 1, material cores 2, solvent tank 3, air inlet pipe 4 and go out
The upper end of tracheae 5, reaction kettle 1 is connected with air inlet pipe 4 and escape pipe 5 respectively, and air inlet pipe 4 is symmetrically connected to the upper end of reaction kettle 1
Both sides, escape pipe 5 are connected to the upper end middle of reaction kettle 1, and lower end and the solvent tank 3 of reaction kettle 1 are connected, and material cores 2 are installed
In the inside of reaction kettle 1；
Heater strip 11 is connected on 1 inner wall of reaction kettle, 1 bottom of reaction kettle is connected with temperature sense meter 12, temperature sense
Temperature probe 121 on meter 12 gos deep between material cores 2, for the temperature in detection reaction kettle 1；
The material cores 2 are interference fitted with 1 inner wall of reaction kettle, and the shape of material cores 2 is " circular comb " shape, and material cores 2 are by described
Novel environment-friendly composite material be made, the cylindrical core on material cores 2 is anti-to improve to increase the contact surface with carbon monoxide
Answer efficiency；
Be contained with reaction dissolvent in the solvent tank 3,3 bottom of solvent tank is connected with solvent pipe 31, solvent pipe 31 with react
The bottom of kettle 1 is connected, and pump 32 and the first solenoid valve 33 are connected in solvent pipe 31；
The air inlet pipe 4 passes through the bottom of 2 intercalation reaction kettle 1 of material cores, air inlet pipe 4 to be interference fitted with material cores 2, air inlet pipe
4 bottom end is equipped with Conic nozzle 41；
The escape pipe 5 is equipped with four-way interface 51, and the first branch pipe 52, the second branch pipe 53 and the are connected on four-way interface 51
Three branch pipes 54 are connected with carbonmonoxide detector 55 on first branch pipe 52, and carbonmonoxide detector 55 is for detecting in escape pipe 5
Carbon monoxide content, one end of the second branch pipe 53 is connected to air inlet pipe 4, and second solenoid valve 56 is connected on the second branch pipe 53,
Third solenoid valve 57 is connected on third branch pipe 54；
Temperature sense meter 12, the 32, first solenoid valve 33 of pump, carbonmonoxide detector 55, second solenoid valve 56 and the third
Network is connect solenoid valve 57 with central controller by radio communication；
The working method of the carbon monoxide absorbing reaction kettle is：Central controller controls open pump 32 and the first solenoid valve
33, reaction dissolvent is passed through in reaction kettle 1, after the liquid level of reaction dissolvent floods material cores 2 completely, closes pump 32 and the first electricity
Magnet valve 33 is opened heater strip 11 and is heated, kept the temperature when the temperature of temperature sense meter 12 is 110-130 DEG C, be passed through an oxidation
Carbon gas opens third solenoid valve 57, and carbon monoxide in an outlet gas is detected every 10min carbonmonoxide detectors 55
Content stop CO gas when carbon monoxide content exceeds setting value and be passed through, close third solenoid valve 57, open
Second solenoid valve 56, while pump 32 and the first solenoid valve 33 withdrawal reaction dissolvent are opened, replace material cores 2.
The above content is just an example and description of the concept of the present invention, affiliated those skilled in the art
It makes various modifications or additions to the described embodiments or substitutes by a similar method, without departing from invention
Design or beyond the scope defined by this claim, be within the scope of protection of the invention.
Claims (8)
1. a kind of novel environment-friendly composite material, it is characterised in that：Each raw material weight percentage is：Chromium trichloride 5-8%, chlordene
Tungsten 5-8%, molybdenum pentachloride 8-12%, alumine hydroxide colloid 10-15%, modified galapectite 60-80%.
2. a kind of novel environment-friendly composite material according to claim 1, it is characterised in that：The system of the modification galapectite
Preparation Method is：Galapectite is added in ball mill and is ground, water is added to be modulated into the galapectite solution of a concentration of 30-35%, side
The concentrated sulfuric acid solution that 45-50% is added in side is stirred, when the pH of clayish solution is 2.3-3.0, stops the addition of the concentrated sulfuric acid, continues
10-15min is stirred, when the pH for measuring galapectite solution again is 2.0-2.5, the clayish solution of acidification is put into water bath sonicator instrument
In, in the case where bath temperature is 60-70 DEG C, ultrasonic 10min takes out supernatant after heat preservation standing at 60-70 DEG C, is obtained by filtration pure
Change galapectite, stops washing when using purifying water washing to pH for 6.5-7.0, the purifying galapectite after washing is put into vacuum and is done
It is -0.01-0.06MPa in vacuum degree in dry case, temperature is dry 24-30h at 62-66 DEG C, the moisture of galapectite to be purified≤
It when 12%, takes out dry purifying galapectite and is put into Muffle furnace, 3-5h is calcined at 900-1000 DEG C, crushed 325 mesh sieve i.e.
The modification galapectite that must be activated.
3. a kind of preparation process of novel environment-friendly composite material, it is characterised in that：Specifically include following steps：
S1, by alumine hydroxide colloid be put into spray drying bed granulation is dried；
S2, alumine hydroxide colloid particle and modified galapectite are put into screw extruder progress melting extrusion, obtained compound porous
Material；
S3, chromium trichloride, tungsten hexachloride and molybdenum pentachloride are added in reactor, under the protection of n-hexane, S2 systems is added
Standby composite porous material is stirred at reflux adsorption reaction 6-8h, filtering, is obtained after 40-50h is dried in vacuo at 55-60 DEG C
Novel environment-friendly composite material.
4. a kind of preparation process of novel environment-friendly composite material according to claim 3, it is characterised in that：Described in step S2
One area's temperature of screw extruder be 120-130 DEG C, two area's temperature of screw extruder be 300-315 DEG C.
5. a kind of preparation process of novel environment-friendly composite material according to claim 3, it is characterised in that：Step S3 is obtained
Novel environment-friendly composite material be applied to carbon monoxide absorbing reaction kettle in carry out carbon monoxide absorption.
6. a kind of preparation process of novel environment-friendly composite material according to claim 5, it is characterised in that：One oxygen
It includes reaction kettle to change carbon absorption reaction kettle（1）, material cores（2）, solvent tank（3）, air inlet pipe（4）And escape pipe（5）, reaction kettle
（1）Upper end respectively with air inlet pipe（4）And escape pipe（5）It connects, air inlet pipe（4）It is symmetrically connected to reaction kettle（1）Upper end two
Side, escape pipe（5）It is connected to reaction kettle（1）Upper end middle, reaction kettle（1）Lower end and solvent tank（3）It connects, material cores
（2）Mounted on reaction kettle（1）Inside；
The reaction kettle（1）Heater strip is connected on inner wall（11）, reaction kettle（1）Bottom is connected with temperature sense meter（12）,
Temperature sense meter（12）On temperature probe（121）Go deep into material cores（2）Between；
The material cores（2）With reaction kettle（1）Inner wall is interference fitted, material cores（2）Shape be " circular comb " shape, material cores
（2）It is made of the novel environment-friendly composite material；
The solvent tank（3）Inside it is contained with reaction dissolvent, solvent tank（3）Bottom is connected with solvent pipe（31）, solvent pipe
（31）With reaction kettle（1）Bottom connect, solvent pipe（31）On be connected with pump（32）With the first solenoid valve（33）；
The air inlet pipe（4）Across material cores（2）Intercalation reaction kettle（1）Bottom, air inlet pipe（4）With material cores（2）Interference
Cooperation, air inlet pipe（4）Bottom end be equipped with Conic nozzle（41）；
The escape pipe（5）It is equipped with four-way interface（51）, four-way interface（51）On be connected with the first branch pipe（52）, second
Pipe（53）With third branch pipe（54）, the first branch pipe（52）On be connected with carbonmonoxide detector（55）, carbonmonoxide detector
（55）For detecting escape pipe（5）In carbon monoxide content, the second branch pipe（53）One end and air inlet pipe（4）Connection, second
Branch pipe（53）On be connected with second solenoid valve（56）, third branch pipe（54）On be connected with third solenoid valve（57）；
The temperature sense meter（12）, pump（32）, the first solenoid valve（33）, carbonmonoxide detector（55）, second solenoid valve
（56）With third solenoid valve（57）Network is connect with central controller by radio communication.
7. a kind of preparation process of novel environment-friendly composite material according to claim 6, it is characterised in that：The reaction
Solvent is N,N-dimethylformamide or dimethyl sulfoxide (DMSO).
8. a kind of preparation process of novel environment-friendly composite material according to claim 6, it is characterised in that：One oxygen
Change carbon absorption reaction kettle working method be：Central controller controls open pump（32）With the first solenoid valve（33）, will react molten
Agent is passed through reaction kettle（1）In, when the liquid level of reaction dissolvent floods material cores completely（2）Afterwards, pump is closed（32）With the first solenoid valve
（33）, open heater strip（11）It is heated, when temperature sense meter（12）Temperature be 110-130 DEG C when keep the temperature, be passed through an oxygen
Change carbon gas, opens third solenoid valve（57）, every 10min carbonmonoxide detectors（55）It detects one in an outlet gas
The content of carbonoxide stops CO gas and is passed through, close third solenoid valve when carbon monoxide content exceeds setting value
（57）, open second solenoid valve（56）, while opening pump（32）With the first solenoid valve（33）Reaction dissolvent is withdrawn, material cores are replaced
（2）.
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