CN104892796B - The streaming separator and method of agricultural-forestry biomass chemical constituent - Google Patents
The streaming separator and method of agricultural-forestry biomass chemical constituent Download PDFInfo
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Abstract
The present invention relates to a kind of streaming separator of agricultural-forestry biomass chemical constituent and method.The separator includes normal temperature solvent holding vessel, thermostat unit, hot solvent holding vessel, extraction tube and collecting tank, normal temperature solvent holding vessel is connected by high-pressure pump with thermostat unit, thermostat unit is connected with hot solvent holding vessel, hot solvent holding vessel is connected by check valve with extraction tube, extraction tube is connected by constant pressure valve with thermostat unit, and thermostat unit is also connected with collecting tank.Using the device, by changing species, temperature, pressure and the flow velocity of solvent, the separation of liposoluble substance in biomass, hemicellulose, lignin and cellulosic component can be realized by the hemicellulose in raw material and lignin fractional extraction into solvent.Separation method of the present invention is that the separation to agricultural-forestry biomass chemical composition is realized under solvent flow state, with separation rapidly and efficiently, solvent usage amount is low, component without degraded the characteristics of.
Description
Technical field
The invention discloses a kind of streaming separator of agricultural-forestry biomass chemical constituent and method, belong to biomass refining
Field.
Background technology
The lignocellulosics such as main stalk, the trees referred in agriculture and forestry production process in addition to grain, fruit of agricultural-forestry biomass,
The material such as farming industry leftover bits and pieces and agriculture and forestry organic waste material, with recyclability, low stain and widely distributed property.Chemically
For composition, biomass contains in addition to containing cellulose, hemicellulose and the big component of lignin three, also containing a certain amount of tree
The liposoluble substances such as fat, fat, wax.
Biomass refining refers to, by the new chemistry of exploitation, biological and mechanical means, convert biomass into as variousization
The set of the technology and equipment of product, fuel and bio-based materials.Efficiently separating for biomass components makes the base of biomass refining
Plinth, can provide suitable raw material, therefore the focus studied as industrial quarters and academia for subsequent transformation.
In recent years, a large amount of patents are emerged in terms of agricultural-forestry biomass chemical constituent separation.Chinese patent document
CN102561082A (application numbers：201210051748.5) disclose a kind of from lignocellulose raw material extraction hemicellulose, fiber
The method of element and lignin, the hemi-cellulose components in hot-water extraction biomass are utilized in static reactor, are then utilized
Alkali organic solvent (containing sodium hydroxide, potassium hydroxide, calcium hydroxide methanol or ethanol solution) extracting lignin component, most
The separation of hemicellulose, lignin and cellulose is realized eventually.Chinese patent document CN102101915A (application numbers：
201010542903.4) a kind of separation method of agricultural-forestry biomass component is disclosed, using ionic liquid by agricultural-forestry biomass powder
Biomass solution all is dissolved as, then using the combination of acetone, water, alkali and ethanol, specific solvent is constituted, biomass is molten
Hemicellulose, cellulose and lignin in liquid respectively are isolated by coming.Chinese patent document CN101790611A (application numbers：
200880102063.0) disclosing one kind, that biomass components are separated into cellulose, hemicellulose and lignin etc. is single
Then the method and system of component, utilized lignin dissolution using 10%~30% ammonia and its derivative in reactor
0.25%-2% inorganic acid is by hemicellulose dissolution, and similar patent also has Chinese patent document CN1779070A (application numbers：
200510036416.X) and Chinese patent document CN103924468A (application numbers：201310688644.X).
But, the separation method described in above-mentioned patent document is realized in a static manner in reactor, less efficient；And
And corrosivity and the stronger solvent of oxidisability such as sodium hydroxide, potassium hydroxide, sulfuric acid, hydrochloric acid, hydrogen peroxide, in static reaction
Extracted in device, the time is longer, carbohydrate degradation is serious, generate the impurity such as substantial amounts of furfural and organic acid, be later
Component purifying bring difficulty.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides streaming separator and the side of a kind of agricultural-forestry biomass chemical constituent
Method, using the apparatus and method, can be achieved the chemical group such as liposoluble substance, hemicellulose, lignin and cellulose in biomass
The quick separating divided.Pass through streaming extracting separation, biomass components outflow reactor while dissolution, it is to avoid the drop of component
Solution, greatly improves the purity of extracting component.
Technical scheme is as follows：
A kind of streaming separator of agricultural-forestry biomass chemical constituent, including normal temperature solvent holding vessel, thermostat unit,
Hot solvent holding vessel, extraction tube and collecting tank, described normal temperature solvent holding vessel are connected by high-pressure pump with thermostat unit,
Described thermostat unit is connected with hot solvent holding vessel, and described hot solvent holding vessel is connected by check valve and extraction tube
Connect, described extraction tube is connected by constant pressure valve with thermostat unit, described thermostat unit also connects with collecting tank
Connect.
, according to the invention it is preferred to, described thermostat unit includes the heater and cooler being connected in parallel, described
Heater be connected respectively with high-pressure pump and hot solvent holding vessel, described cooler connects with constant pressure valve and collecting tank respectively
Connect.
, according to the invention it is preferred to, it is additionally provided with pressure gauge between described constant pressure valve and extraction tube.
, according to the invention it is preferred to, described extraction tube is internally provided with helixes feed equipment, the charging aperture of extraction tube and
Discharging opening is provided with filter screen.Filter screen is used to prevent the loss of agricultural-forestry biomass material.
, according to the invention it is preferred to, described high-pressure pump is polynary gradient high-pressure pump, can realize times of 2~4 kinds of solvents
Meaning volume mixture, using the teaching of the invention it is possible to provide 1~40MPa constant pressure；
It is preferred that, the temperature regulating range of described thermostat unit is at 10~400 DEG C；
It is preferred that, described constant pressure valve can be adjusted pressure between 1~40MPa.
According to the present invention, a kind of streaming separation method of agricultural-forestry biomass chemical constituent, including the use of said apparatus, including
Step is as follows；
(1) it is fitted into after agricultural-forestry biomass raw material is crushed in extraction tube, solvent is fitted into normal temperature solvent holding vessel, passed through
Solvent is pumped into thermostat unit by high-pressure pump, and the heater in thermostat unit is transported to hot solvent after solvent is heated
In holding vessel, the flow velocity of regulation check valve and constant pressure valve control solvent and then solvent is controlled in the residence time of extraction tube, it is molten
Agent is extracted to agricultural-forestry biomass chemical constituent；
Pressure in high-pressure pump regulation extraction process is 1~40MPa；
(2) extract after terminating, extract the solvent after chemical constituent and enter in thermostat unit, in thermostat unit
Condenser is condensed to solvent and is transported to normal temperature in collecting tank, and solvent evaporative removal is produced into agricultural-forestry biomass chemical constituent.
, according to the invention it is preferred to, in step (1), when separating the liposoluble substance in agricultural-forestry biomass, described is molten
Agent is benzene, toluene, methanol, ethanol, supercritical carbon dioxide or/and methyl tertiary butyl ether(MTBE), and the temperature after solvent heating is 40-
210 DEG C, pressure 0.5-25MPa, solvent is 5-120min in the residence time of extraction tube；It is further preferred that described liposoluble
Property material is including but not limited to resin, vegatable tannin, aliphatic acid, phytosterol；It is furthermore preferred that the temperature after solvent heating is
100-120 DEG C, pressure 6-8MPa, solvent is 20-40min in the residence time of extraction tube；
When separating the hemicellulose in agricultural-forestry biomass, described solvent is water, the diluted acid of 0.2-10wt% concentration is molten
Liquid, the temperature after solvent heating is 100-190 DEG C, pressure 2.5-10MPa, and solvent is 2-60min in the residence time of extraction tube；
It is further preferred that described dilute acid soln is sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid or carbonic acid；It is furthermore preferred that described solvent is
The dilute acid soln of water, 0.1-2wt% concentration, the temperature after solvent heating is 160-180 DEG C, pressure 6-8MPa, and solvent is in extracting
The residence time of pipe is 10-30min；
When separating the lignin in agricultural-forestry biomass, described solvent is dilute alkaline soln, the 0.1- of 1-20wt% concentration
Inorganic salt solution, tetrahydrofuran, dioxane, dimethylformamide, dimethyl sulfoxide (DMSO) or/and the liquefied ammonia of 2wt% concentration, solvent
Temperature after heating is 80-180 DEG C, pressure 0.5-25MPa, and solvent is 10-90min in the residence time of extraction tube；Further
It is preferred that, described dilute alkaline soln is sodium hydroxide, potassium hydroxide, calcium hydroxide, and described inorganic salts are carbonate or sulfurous
Hydrochlorate；It is furthermore preferred that described solvent is the dilute alkaline soln of 6-8wt% concentration, the inorganic salt solution of 0.1-0.5wt% concentration,
Tetrahydrofuran, dioxane, dimethylformamide, dimethyl sulfoxide (DMSO) or/and liquefied ammonia, the temperature after solvent heating are 80-140
DEG C, pressure 6-15MPa, solvent is 10-30min in the residence time of extraction tube；
It is preferred that, the pressure in high-pressure pump regulation extraction process is 8~30MPa；
It is preferred that, described solvent and the mass ratio of agricultural-forestry biomass raw material are 3-15:1.
, according to the invention it is preferred to, described agricultural-forestry biomass raw material is poplar.
According to the present invention, agricultural-forestry biomass raw material is fitted into extraction tube, solvent is flowed in extraction tube using high-pressure pump
It is dynamic, by controlling species, ratio, temperature, pressure and the flow velocity of solvent, by the liposoluble substance in agricultural-forestry biomass raw material, half
Cellulose, lignin component are extracted into solvent successively, and cellulosic component is final in agricultural-forestry biomass exists in the form of solid-state
In extraction tube, the separation of biomass chemical constituent is realized.
Beneficial effects of the present invention：
1st, separator of the present invention is simple in construction, uses light, good separating effect.
2nd, separation method of the present invention is that the separation to agricultural-forestry biomass chemical composition is realized under solvent flow state, is had
Separation is rapidly and efficiently, solvent usage amount is low, component without degraded the characteristics of.
Brief description of the drawings
Fig. 1 is the agent structure schematic diagram of the streaming separator of agricultural-forestry biomass chemical constituent of the present invention；Wherein：1st, often
Warm solvent holding vessel, 2, high-pressure pump, 3, thermostat unit, 4, hot solvent holding vessel, 5, check valve, 6, extraction tube, 7, pressure
Table, 8, constant pressure valve, 9, collecting tank.
Embodiment
Below by specific embodiment, the present invention will be further described, but not limited to this.
Embodiment 1：
A kind of streaming separator of agricultural-forestry biomass chemical constituent, including normal temperature solvent holding vessel 1, thermostat unit
3rd, hot solvent holding vessel 4, extraction tube 6 and collecting tank 9, described normal temperature solvent holding vessel 1 pass through high-pressure pump 2 and temperature adjustment list
Member 3 is connected, and described thermostat unit 3 is connected with hot solvent holding vessel 4, and described hot solvent holding vessel 4 passes through check valve 5
It is connected with extraction tube 6, described extraction tube 6 is connected by constant pressure valve 8 with thermostat unit 3, described temperature adjustment list
Member 3 is also connected with collecting tank 9；
Described thermostat unit 3 includes the heater and cooler that are connected in parallel, described heater respectively with height
Press pump 2 and hot solvent holding vessel 4 are connected, and described cooler is connected with constant pressure valve 8 and collecting tank 9 respectively；
Pressure gauge 7 is additionally provided between described constant pressure valve 8 and extraction tube 6；
Described extraction tube 6 is internally provided with helixes feed equipment, and the charging aperture and discharging opening of extraction tube 6 are provided with filter
Net；
Described high-pressure pump 2 is polynary gradient high-pressure pump, can realize the arbitrary volume mixing of 2~4 kinds of solvents, Neng Gouti
For 1~40MPa constant pressure；
The temperature regulating range of described thermostat unit 3 is at 10~400 DEG C；
Described constant pressure valve 8 can be adjusted pressure between 1~40MPa.
Embodiment 2：
A kind of described device of utilization embodiment 1 is as follows to the streaming separation method of poplar chemical constituent, including step；
(1) it is fitted into after poplar raw material is crushed in extraction tube 6, solvent is fitted into normal temperature solvent holding vessel 1, passes through high pressure
Solvent is pumped into thermostat unit 3 by pump 2, and the heater in thermostat unit 3 is transported to hot solvent after solvent is heated
In holding vessel 4, the flow velocity and then control solvent of regulation check valve 5 and the control solvent of constant pressure valve 8 are in the stop of extraction tube 6
Between, solvent is extracted to agricultural-forestry biomass chemical constituent；
The separation of different chemical constituents is realized using different solvents, it is specific as follows：
A, solvent are methyl tertiary butyl ether(MTBE), and the heated solvent temperature of thermostat unit 3 is to 100-110 DEG C, and regulation flow velocity makes
Residence time 30min of the solvent in extraction tube 6, persistently pumps 60min, using 4 times that solvent quality is poplar material quality,
Obtain the t-butyl methyl ether solution containing liposoluble substance (resin, vegatable tannin, aliphatic acid and phytosterol)；
B, solvent are water, and the heated solvent temperature of thermostat unit 3 is to 175-185 DEG C, and regulation flow velocity makes solvent in extracting
Residence time 20min in pipe 6, persistently pumps 40min, using 4 times that solvent quality is poplar material quality, obtains containing half
The aqueous solution of cellulose；
C, solvent are tetrahydrofuran solution, and the heated solvent temperature of thermostat unit 3 is to 120-135 DEG C, and regulation flow velocity makes
Residence time 20min of the solvent in extraction tube 6, persistently pumps 60min, using 4 times that solvent quality is poplar material quality,
Obtain the tetrahydrofuran solution containing lignin；
Pressure in the regulation extraction process of high-pressure pump 2 is 8~30MPa；
(2) extract after terminating, extract the solvent after chemical constituent and enter in thermostat unit 3, in thermostat unit 3
Condenser solvent condensed to normal temperature be transported in collecting tank 9；
Evaporative removal methyl tertiary butyl ether(MTBE) is dried to obtain hemicellulose after obtaining liposoluble substance, evaporative removal water, evaporation
Remove tetrahydrofuran solution and obtain lignin, the solid taken out in extraction tube 6 obtains cellulose.
In the present embodiment, the yield of liposoluble substance is 95-99%, and the yield of hemicellulose is 75-90%, lignin
Yield is 86-95%, and cellulose yield is 80-96%.In addition, not detecting furfural and hydroxyl in the above-mentioned hemicellulose aqueous solution
The catabolite of the sugar such as methyl furfural.
Comparative example：
The static separation of poplar raw material chemical constituent, including step are as follows：
It is put into after poplar raw material is crushed in reactor, and adds the methyl tertiary butyl ether(MTBE) of 6 times of poplar material qualities, heating
To 100-110 DEG C and maintain 30min, cool tapping, obtains containing liposoluble substance (resin, fat, wax and phytosterol)
T-butyl methyl ether solution, evaporative removal t-butyl methyl ether solution obtains liposoluble substance.
The water of 6 times of poplar material qualities is added into reactor, 175-185 DEG C is heated to and maintains 20min, cooling is put
Liquid, obtains the aqueous solution containing hemicellulose, and evaporative removal water is simultaneously dried to obtain hemicellulose.
The tetrahydrofuran of 6 times of poplar material qualities of sawdust is added into reactor, 120-135 DEG C is heated to and is incubated
20min, cool tapping, obtains the tetrahydrofuran solution containing lignin, evaporative removal tetrahydrofuran obtains lignin.
The solid residue in reactor is finally taken out, cellulose is obtained.
In this comparative example, the yield of liposoluble substance is 85-90%, and the yield of hemicellulose is 45-60%, lignin
Yield is 50-64%, and cellulose yield is 70-82%.In addition, not detecting 2-5g/L chaffs in the above-mentioned hemicellulose aqueous solution
The catabolite of the sugar such as aldehyde and 1-3g/L hydroxymethylfurfurals.
Pass through comparative example 1 and comparative example, it is known that, streaming separation method of the invention is separated than static type separation method
Efficiency is significantly improved, and carbohydrate is not degraded.
Embodiment 3：
A kind of described device of utilization embodiment 1 is as follows to the streaming separation method of poplar chemical constituent, including step；
(1) it is fitted into after poplar raw material is crushed in extraction tube 6, solvent is fitted into normal temperature solvent holding vessel 1, passes through high pressure
Solvent is pumped into thermostat unit 3 by pump 2, and the heater in thermostat unit 3 is transported to hot solvent after solvent is heated
In holding vessel 4, the flow velocity and then control solvent of regulation check valve 5 and the control solvent of constant pressure valve 8 are in the stop of extraction tube 6
Between, solvent is extracted to agricultural-forestry biomass chemical constituent；
The separation of different chemical constituents is realized using different solvents, it is specific as follows：
A, solvent are ethanol, and the heated solvent temperature of thermostat unit 3 is to 100-110 DEG C, and regulation flow velocity is taking out solvent
The residence time 30min in pipe 6 is carried, 60min is persistently pumped, using 4 times that solvent quality is poplar material quality, is contained
The ethanol solution of liposoluble substance (resin, vegatable tannin, aliphatic acid and phytosterol)；
B, solvent are 0.2wt% hydrochloric acid, and the heated solvent temperature of thermostat unit 3 is to 175-185 DEG C, and regulation flow velocity makes
Residence time 10min of the solvent in extraction tube 6, persistently pumps 40min, using 4 times that solvent quality is poplar material quality,
Obtain the hydrochloric acid solution containing hemicellulose；
C, solvent are the dioxane aqueous solution (90.2% dioxane, 9.8% water), the heated solvent of thermostat unit 3
Temperature is to 80-120 DEG C, and regulation flow velocity makes residence time 20min of the solvent in extraction tube 6,40min is persistently pumped, using molten
Agent quality is 4 times of poplar material quality, obtains the dioxane aqueous solution containing lignin；
Pressure in the regulation extraction process of high-pressure pump 2 is 8~30MPa；
(2) extract after terminating, extract the solvent after chemical constituent and enter in thermostat unit 3, in thermostat unit 3
Condenser solvent condensed to normal temperature be transported in collecting tank 9；
Evaporative removal ethanol is dried to obtain hemicellulose after obtaining liposoluble substance, evaporative removal hydrochloric acid, and evaporative removal is molten
Liquid obtains lignin, and the solid taken out in extraction tube 6 obtains cellulose.
In the present embodiment, the yield of liposoluble substance is 95-99%, and the yield of hemicellulose is 70-80%, lignin
Yield is 90-95%, and cellulose yield is 90-95%.
Embodiment 4：
As described in Example 2, unlike：
In step (1), A, solvent are toluene, and the heated solvent temperature of thermostat unit 3 adjusts flow velocity to 100-110 DEG C
Make residence time 20min of the solvent in extraction tube 6, persistently pump 40min, use 6 that solvent quality is poplar material quality
Times, obtain the toluene solution containing liposoluble substance (resin, vegatable tannin, aliphatic acid and phytosterol)；
B, solvent are 0.2wt% sulfuric acid, and the heated solvent temperature of thermostat unit 3 is to 175-185 DEG C, and regulation flow velocity makes
Residence time 20min of the solvent in extraction tube 6, persistently pumps 40min, using 6 times that solvent quality is poplar material quality,
Obtain the sulfuric acid solution containing hemicellulose；
C, solvent are 0.2wt% sodium hydroxide solutions, and the heated solvent temperature of thermostat unit 3 is to 110-120 DEG C, regulation
Flow velocity makes residence time 30min of the solvent in extraction tube 6, persistently pumps 40min, the use of solvent quality is poplar material quality
4 times, obtain the sodium hydroxide solution containing lignin；
In step (2), after extraction terminates, extract the solvent after chemical constituent and enter in thermostat unit 3, temperature adjustment
Condenser in unit 3 is condensed to normal temperature to solvent to be transported in collecting tank 9；
Evaporative removal toluene is dried to obtain hemicellulose after obtaining liposoluble substance, evaporative removal solution, and evaporative removal is molten
Liquid obtains lignin, and the solid taken out in extraction tube 6 obtains cellulose.
Claims (8)
1. a kind of streaming separator of agricultural-forestry biomass chemical constituent, it is characterised in that the agricultural-forestry biomass chemical constituent
Streaming separator includes normal temperature solvent holding vessel, thermostat unit, hot solvent holding vessel, extraction tube and collecting tank, described
Normal temperature solvent holding vessel be connected by high-pressure pump with thermostat unit, described thermostat unit and hot solvent holding vessel
Connection, described hot solvent holding vessel is connected by check valve with extraction tube, and described extraction tube passes through constant pressure valve and temperature
Adjustment unit is connected, and described thermostat unit is also connected with collecting tank；
Described thermostat unit includes the heater and cooler that are connected in parallel, described heater respectively with high-pressure pump and
Hot solvent holding vessel is connected, and described cooler is connected with constant pressure valve and collecting tank respectively；
Described extraction tube is internally provided with helixes feed equipment, and the charging aperture and discharging opening of extraction tube are provided with filter screen；
Described high-pressure pump is polynary gradient high-pressure pump.
2. the streaming separator of agricultural-forestry biomass chemical constituent according to claim 1, it is characterised in that described perseverance
Pressure gauge is additionally provided between pressure valve and extraction tube.
3. the streaming separator of agricultural-forestry biomass chemical constituent according to claim 1, it is characterised in that described height
It is 1 ~ 40MPa that press pump, which provides pressure limit,.
4. the streaming separator of agricultural-forestry biomass chemical constituent according to claim 1, it is characterised in that described temperature
The temperature regulating range of adjustment unit is spent at 10 ~ 400 DEG C.
5. a kind of streaming separation method of agricultural-forestry biomass chemical constituent, including the use of the stream described in claim any one of 1-4
Formula separator, including step are as follows；
（1）It is fitted into after agricultural-forestry biomass raw material is crushed in extraction tube, solvent is fitted into normal temperature solvent holding vessel, passes through high pressure
Solvent is pumped into thermostat unit by pump, and the heater in thermostat unit is transported to hot solvent storage after solvent is heated
In tank, the flow velocity and then control solvent of regulation check valve and constant pressure valve control solvent are in the residence time of extraction tube, solvent pair
Agricultural-forestry biomass chemical constituent is extracted；
Pressure in high-pressure pump regulation extraction process is 1 ~ 40MPa；
（2）After extraction terminates, extract the solvent after chemical constituent and enter in thermostat unit, the condensation in thermostat unit
Device is condensed to solvent and is transported to normal temperature in collecting tank, and solvent evaporative removal is produced into agricultural-forestry biomass chemical constituent.
6. the streaming separation method of agricultural-forestry biomass chemical constituent according to claim 5, it is characterised in that step（1）
In, when separating the liposoluble substance in agricultural-forestry biomass, described solvent is benzene, toluene, methanol, ethanol, overcritical dioxy
Change carbon or/and methyl tertiary butyl ether(MTBE), the temperature after solvent heating is 40-210 DEG C, pressure 0.5-25MPa, and solvent is in extraction tube
Residence time is 5-120min；Described liposoluble substance is resin, vegatable tannin, aliphatic acid, phytosterol；After solvent heating
Temperature be 100-120 DEG C, pressure 6-8 MPa, solvent extraction tube residence time be 20-40min；
When separating the hemicellulose in agricultural-forestry biomass, described solvent is water, the dilute acid soln of 0.2-10wt% concentration, molten
Temperature after agent heating is 100-190 DEG C, pressure 2.5-10MPa, and solvent is 2-60min in the residence time of extraction tube；It is described
Dilute acid soln be sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid or carbonic acid；
When separating the lignin in agricultural-forestry biomass, described solvent is dense for dilute alkaline soln, the 0.1-2wt% of 1-20wt% concentration
Inorganic salt solution, tetrahydrofuran, dioxane, dimethylformamide, dimethyl sulfoxide (DMSO) or/and the liquefied ammonia of degree, after solvent heating
Temperature be 80-180 DEG C, pressure 0.5-25MPa, solvent extraction tube residence time be 10-90min；Described diluted alkaline is molten
Liquid is sodium hydroxide, potassium hydroxide, calcium hydroxide, and described inorganic salts are carbonate or sulphite.
7. the streaming separation method of agricultural-forestry biomass chemical constituent according to claim 5, it is characterised in that step（1）
Described in the mass ratio of solvent and agricultural-forestry biomass raw material be 3-15:1.
8. the streaming separation method of agricultural-forestry biomass chemical constituent according to claim 5, it is characterised in that step（1）
Described in agricultural-forestry biomass raw material be poplar.
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