CN105820312B - A kind of Chinese medicine dreg prepares the preparation method of epoxy resin - Google Patents
A kind of Chinese medicine dreg prepares the preparation method of epoxy resin Download PDFInfo
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- CN105820312B CN105820312B CN201610301615.7A CN201610301615A CN105820312B CN 105820312 B CN105820312 B CN 105820312B CN 201610301615 A CN201610301615 A CN 201610301615A CN 105820312 B CN105820312 B CN 105820312B
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- 239000003814 drug Substances 0.000 title claims abstract description 32
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 28
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 238000000605 extraction Methods 0.000 claims abstract description 18
- 238000004880 explosion Methods 0.000 claims abstract description 14
- 229920005610 lignin Polymers 0.000 claims abstract description 13
- 239000001913 cellulose Substances 0.000 claims abstract description 11
- 229920002678 cellulose Polymers 0.000 claims abstract description 11
- 239000000284 extract Substances 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 239000000047 product Substances 0.000 claims description 20
- 238000001914 filtration Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000002023 wood Substances 0.000 claims description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 12
- 239000000835 fiber Substances 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000005422 blasting Methods 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical class [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000012265 solid product Substances 0.000 claims description 6
- 230000015556 catabolic process Effects 0.000 claims description 5
- 238000006731 degradation reaction Methods 0.000 claims description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000006837 decompression Effects 0.000 claims description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 238000012423 maintenance Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 239000003643 water by type Substances 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 241000756943 Codonopsis Species 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- YWNYZQTZOONLGU-UHFFFAOYSA-N C(CC)Cl.[O] Chemical compound C(CC)Cl.[O] YWNYZQTZOONLGU-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007327 hydrogenolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229920001542 oligosaccharide Polymers 0.000 description 1
- 150000002482 oligosaccharides Chemical class 0.000 description 1
- 239000003895 organic fertilizer Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/02—Polycondensates containing more than one epoxy group per molecule
- C08G59/04—Polycondensates containing more than one epoxy group per molecule of polyhydroxy compounds with epihalohydrins or precursors thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G1/00—Lignin; Lignin derivatives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Dry Formation Of Fiberboard And The Like (AREA)
- Epoxy Resins (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses the preparation method that a kind of Chinese medicine dreg prepares epoxy resin, it is made through following three step：When lignin and cellulose in steam explosion extraction Chinese medicine dreg, second, the hydrogenation of lignin and cellulose is degraded, third, the preparation of epoxy resin.It is raw material that this method, which make use of the Chinese medicine dreg after explosion, extracts product respectively and prepares the synthesis material of epoxy resin, finally obtains epoxy resin with epichlorohydrin reaction.By above-mentioned steps, product epoxy resin is obtained, have has that very strong chemical resistance, mechanical strength are high, electrical insulating property is good, the property such as corrosion-resistant well.
Description
Technical field
The present invention is to be related to the synthesis that the new technology steam explosion of organic matter is carried out to product, product rich in cellulose and
Lignin, to prepare epoxy resin.
Background technology
Chinese medicine dreg from Chinese patent drug production, Chinese medicine processing with processings, production of raw medicine etc., with Chinese patent drug production band
The dregs of a decoction amount come is maximum, accounts for the 70% of dregs of a decoction total amount.With developing rapidly for traditional Chinese medicine, China turns into Chinese medicine in the world
The big country of production, the processing of the dregs of a decoction is also a great problem, the discarded amount benefit increase of Chinese medicine slag of major herbal pharmaceutical factory, annual emissions
Up to 30,000,000 tons.Most of these Chinese medicine slags are considered as waste discharge or landfill falls, and on the one hand cause the pole of resource
It is big to waste；On the other hand, dregs of a decoction accumulation in the wild, due to the shower of rainwater, can rot, the environment to surrounding is made very big
Pollution, therefore the processing of Chinese medicine dreg is extremely urgent.
Substantially have as culture matrix in Chinese medicine dreg processing at present, as some animal feeds, as organic fertilizer
Deng there is potential commercial significance using Chinese medicine dreg as chemically composited synthetic material.These modes not only avoid environment dirt
Dye also improves the utilization rate of resource.Do not show that Chinese medicine dreg synthetic epoxy resin etc. is studied in existing material.
Lignin and oligosaccharide, synthetic epoxy resin are produced by Chinese medicine dreg blasting method, are a kind of green to discarded object
The processing method of color.The present invention to Chinese medicine dreg, carries out explosion degraded by steam explosion technology, and after integrating dregs of a decoction explosion
Product formation epoxy resin, rationally it is preferably minimized waste residue using raw material, to produce epoxy resin, very with potentiality.This hair
Bright to make use of Radix Codonopsis or Radix Angelicae Sinensis Chinese medicine dreg, reaction has obtained epoxy resin.
The content of the invention
Present invention solves the technical problem that it is in view of the shortcomings of the prior art, there is provided a kind of Chinese medicine dreg prepares epoxy resin
Preparation method.
The purpose of the present invention is achieved through the following technical solutions：A kind of Chinese medicine dreg prepares the preparation side of epoxy resin
Method, carry out as follows：
(1) lignin and cellulose in steam explosion extraction Chinese medicine dreg：
(1.1) 100g Chinese medicine dregs are put into steam blasting device, successively under the pressure of 35,45 and 55 atmospheric pressure
Demolition set temperature equipped with the dregs of a decoction is heated to 100-350 DEG C, wherein, keep 5min under each pressure value；Then will reaction
Pressure in device reduces to 1 atmospheric pressure, completes explosion.
(1.2) rugose wood element extraction：The dregs of a decoction after 5g step 1 explosions are taken, are added in 100mL distilled water, are stirred
24h.It is separated by filtration, obtains solid residue.Solid residue is soaked into 24h with methanol at room temperature, is separated by filtration, filtrate is carried out
Concentration, obtain rugose wood element.
(1.3) crude fibre extracts：According to step 1.2 extraction rugose wood element, extraction is then followed the steps below：
(1.3) crude fibre extracts：According to step 1.2 extraction rugose wood element, extraction is then followed the steps below：
(1.3.1) soaks rugose wood element 4 hours with 15mL liquefied ammonia, is separated by filtration, by filtrate (i.e. ammonia soluble substance)
It is placed in reactor, then xeothermic 1h at 100 DEG C, collects solid product；Filter residue is moved into 250mL conical flasks, adds 65mL
Distilled water, 0.5mL glacial acetic acid, 0.6g sodium chlorites, shake up；
(1.3.2) takes 25mL conical flasks, by its back-off in the opening of 250mL conical flasks, then puts 250mL conical flasks
1h is heated in 75 DEG C of waters bath with thermostatic control.
(1.3.3) adds 0.5mL glacial acetic acid and 0.6g sodium chlorites into 250mL conical flasks, after buckling 25mL conical flasks,
Continuation heats 1h in 75 DEG C of water-baths；
(1.3.4) repeat step 1.3.3 is carried out 3-4 times, terminates reaction；After being cooled to room temperature, suction filtration, filter residue is used
Distilled water washs to neutrality repeatedly, puts in 105 scholar, 2 DEG C of baking ovens and dries to constant weight.
The solid product that (1.3.5) combining step 1.3.1 and step 1.3.4 are obtained, that is, obtain the mixture of crude fibre.
(2) hydrogenation of lignin and cellulose is degraded：By 12g rugose woods element or 12g crude fibres and 100m1 absolute ethyl alcohols
After well mixed, 4gNi catalyst is added, is transferred in autoclave.Nitrogen is passed through into reactor, to remove reactor
Interior air, then passes to hydrogen, is reacted under 4Mpa pressure.The reaction solution in reactor is carried out by magnetic stirring apparatus
Stirring, and it is 120 DEG C, mixing speed 900-1000r/min, mixing time 4h to keep reactor temperature.Natural cooling
To room temperature, by reacted liquid Filtration of catalyst, filtrate steams alcohol solvent, product after being degraded.
(3) preparation of epoxy resin：By the mixing of product of the product after 11.4g lignin degradations after cellulose degradation
Thing (mass ratio 1:1), 46.5g epoxychloropropane, 0.25~0.5mL distilled water is well mixed to be added in 500mL there-necked flasks.Claim
4.1gNaOH is taken, the NaOH of l/10 amounts (0.41g) is first added under agitation, is heated to 80~90 DEG C, exothermic heat of reaction simultaneously has
NaCl is generated.Maintenance reaction temperature is at 90 DEG C.1/10 amount (0.41g) NaOH is added after 10min, is added later every 10min
NaOH, adds 1/10 (0.41g) of NaOH total amounts every time, until 4.1gNaOH is added.Continue to terminate after reacting 25min
Reaction, obtains reaction solution.At 60-70 DEG C, reacting liquid filtering is removed into accessory substance NaCl, excessive ring is distilled off under decompression
Oxygen chloropropane, that is, obtain epoxy resin.
The beneficial effects of the present invention are：The new utilization ways of the dregs of a decoction are explored, by the substantial amounts of dregs of a decoction of steam blasting,
Separation and Extraction blast products, green syt epoxy resin.Whole synthesis flow has used the thought of Green Chemistry, and product has work
Industry applying value, very with potentiality.
Brief description of the drawings
Accompanying drawing 1 is the Technology Roadmap that Chinese medicine dreg of the present invention prepares epoxy resin；
Accompanying drawing 2 is Radix Codonopsis Chinese medicine dreg infrared absorpting light spectra of the present invention；
Accompanying drawing 3 is steam blasting device commonly used in the art；
Accompanying drawing 4 is hydrogenolysis device commonly used in the art.
Embodiment
First buy the following raw material：Buy methanol, liquefied ammonia, Ni catalyst, toluene, sodium sulphate, H2, epoxychloropropane, hydrogen-oxygen
Change sodium, the present embodiment makees unit of weight with g.
The present invention is with reference to embodiment and is further elaborated referring to the drawings：
Embodiment:
(1) (the Radix Angelicae Sinensis dregs of a decoction) prepare epoxy resin, meet epoxy resin national standard, can reach high-class product standard.
(2) (the Radix Codonopsis dregs of a decoction) prepare epoxy resin, meet epoxy resin national standard, can reach high-class product standard.
(1) extraction of Chinese medicine dreg (Radix Codonopsis or Radix Angelicae Sinensis) steam blasting lignin：
(1.1) 100g Chinese medicine dregs (Radix Codonopsis or Radix Angelicae Sinensis) are put into steam blasting device, it is big at 35,45 and 55 successively
The demolition set temperature equipped with the dregs of a decoction is heated to 100-350 DEG C under the pressure of air pressure, wherein, kept under each pressure value
5min；Then the pressure in reactor is reduced into 1 atmospheric pressure, completes explosion.
(1.2) rugose wood element extraction：The dregs of a decoction after 5g step 1 explosions are taken, are added in 100mL distilled water, are stirred
24h.It is separated by filtration, obtains solid residue.Solid residue is soaked into 24h with methanol at room temperature, is separated by filtration, filtrate is carried out
Concentration, obtain rugose wood element.
(1.3) crude fibre extracts：According to step 1.2 extraction rugose wood element, extraction is then followed the steps below：
(1.3) crude fibre extracts：According to step 1.2 extraction rugose wood element, extraction is then followed the steps below：
(1.3.1) soaks rugose wood element 4 hours with 15mL liquefied ammonia, is separated by filtration, by filtrate (i.e. ammonia soluble substance)
It is placed in reactor, then xeothermic 1h at 100 DEG C, collects solid product；Filter residue is moved into 250mL conical flasks, adds 65mL
Distilled water, 0.5mL glacial acetic acid, 0.6g sodium chlorites, shake up；
(1.3.2) takes 25mL conical flasks, by its back-off in the opening of 250mL conical flasks, then puts 250mL conical flasks
1h is heated in 75 DEG C of waters bath with thermostatic control.
(1.3.3) adds 0.5mL glacial acetic acid and 0.6g sodium chlorites into 250mL conical flasks, after buckling 25mL conical flasks,
Continuation heats 1h in 75 DEG C of water-baths；
(1.3.4) repeat step 1.3.3 is carried out 3-4 times, terminates reaction；After being cooled to room temperature, suction filtration, filter residue is used
Distilled water washs to neutrality repeatedly, puts in 105 scholar, 2 DEG C of baking ovens and dries to constant weight.
The solid product that (1.3.5) combining step 1.3.1 and step 1.3.4 are obtained, that is, obtain the mixture of crude fibre.
(2) hydrogenation of lignin and cellulose is degraded：12g lignin degradation products and 12g cellulose degradations are weighed respectively
Product is put into two reactors and is separately added into 4gNi catalyst, is dissolved and is stirred with 100m1 absolute ethyl alcohols in beaker
Afterwards, it is transferred in autoclave.Nitrogen cylinder is opened, air is removed, is passed through hydrogen, is reacted under 4Mpa pressure.Open
Condensed water, start agitator and adjust stir speed (S.S.), and keep reactor temperature be 120 DEG C, it is to be heated to reaction temperature when,
Adjustment mixing speed starts clock reaction, mixing speed 900-1000r/min, mixing time 4h.Kept in course of reaction
Reaction temperature is constant.Stop heating after the completion of reaction, naturally cool to room temperature.By reacted liquid Filtration of catalyst,
Solution steams alcohol solvent, product after being degraded.
(3) preparation of epoxy resin：Agitator is installed on 500mL there-necked flasks, returns condenser pipe and thermometer.Add
11.4g ratios are 1:1 lignocellulose mixture, 46.5g epoxychloropropane, 0.25~0.5mL distilled water.Weigh
4.1gNaOH, the NaOH for first adding l/10 amounts start stirring, are slowly heated to 80~90 DEG C.Exothermic heat of reaction simultaneously has NaCl generations.
Maintenance reaction temperature is at 90 DEG C.The NaOH of 1/10 amount is added after about 10min, adds a NaOH every 10min later, every time
Add the 1/10 of NaOH total amounts, until 4.1gNaOH is added.Continue to terminate reaction after reacting 25min.Product is light yellow.
Reacting liquid filtering is removed accessory substance NaCl by 60-70 DEG C, and excessive epoxychloropropane (recovery) is distilled off under decompression.Stop steaming
Evaporate, residue is poured into small beaker while hot, obtains faint yellow, transparent, sticky product, course of reaction is as follows.
The infared spectrum of resulting product is as shown in Fig. 2 yield about 15g.As can be seen from Figure 2 in 815cm-1Left and right
There is epoxy radicals characteristic peak, in 1116cm-1There is obvious ehter bond absworption peak, in 1364cm-1Place's absworption peak disappears substantially can be with
Most phenolic hydroxyl group fundamental reaction is found out, in 1214cm-1The absworption peak at place represents aromatic series C-O stretching vibration,
1510cm-1There is the characteristic peak of phenyl ring in place, and the product that can be proved to obtain from above is epoxy resin.
The testing result of products therefrom is as shown in the table.
Claims (1)
1. a kind of Chinese medicine dreg prepares the preparation method of epoxy resin, it is characterized in that, carry out as follows：
（1）Lignin and cellulose in steam explosion extraction Chinese medicine dreg：
（1.1）100g Chinese medicine dregs are put into steam blasting device, successively will dress under the pressure of 35,45 and 55 atmospheric pressure
The demolition set temperature for having the dregs of a decoction is heated to 100-350 DEG C, wherein, keep 5min under each pressure value；Then by reactor
Pressure reduce to 1 atmospheric pressure, complete explosion；
（1.2）Rugose wood element extraction：The dregs of a decoction after 5g step 1 explosions are taken, are added in 100mL distilled water, stir 24h；Cross
Filter separation, obtains solid residue；Solid residue is soaked into 24h with methanol at room temperature, is separated by filtration, filtrate is concentrated,
Obtain rugose wood element；
（1.3）Crude fibre extracts：According to step 1.2 extraction rugose wood element, extraction is then followed the steps below：
（1.3.1）Rugose wood element is soaked 4 hours with 15mL liquefied ammonia, is separated by filtration, filtrate is placed in reactor, then
Xeothermic 1h at 100 DEG C, collect solid product；Filter residue is moved into 250 mL conical flasks, adds 65 mL distilled water, 0.5 mL ice
Acetic acid, 0.6 g sodium chlorites, shakes up；
（1.3.2）25mL conical flasks are taken, by its back-off in the opening of 250 mL conical flasks, are then placed in 250 mL conical flasks
1h is heated in 75 DEG C of waters bath with thermostatic control；
（1.3.3）0.5 mL glacial acetic acid and 0.6g sodium chlorites are added into 250 mL conical flasks, after buckling 25mL conical flasks, after
Continue and heat 1h in 75 DEG C of water-baths；
（1.3.4）Repeat step 1.3.3 is carried out 3-4 times, terminates reaction；After being cooled to room temperature, suction filtration, filter residue is distilled
Water washs to neutrality repeatedly, puts in 105 ± 2 DEG C of baking ovens and dries to constant weight；
（1.3.5）The solid product that combining step 1.3.1 and step 1.3.4 are obtained, that is, obtain the mixture of crude fibre；
（2）The hydrogenation of lignin and cellulose is degraded：12g rugose woods element or 12g crude fibres and 100m1 absolute ethyl alcohols are mixed
After uniformly, 4gNi catalyst is added, is transferred in autoclave；Nitrogen is passed through into reactor, to remove in reactor
Air, hydrogen is then passed to, reacted under 4Mpa pressure；The reaction solution in reactor is stirred by magnetic stirring apparatus
Mix, and it is 120 DEG C, mixing speed 900-1000r/min, mixing time 4h to keep reactor temperature；Naturally cool to
Room temperature, by reacted liquid Filtration of catalyst, filtrate steams alcohol solvent, product after being degraded；
（3）The preparation of epoxy resin：By the product after the product and cellulose degradation after 11.4g lignin degradations according to mass ratio
1:The mixture of 1 composition, 46.5g epoxychloropropane, 0.25~0.5mL distilled water is well mixed to be added in 500mL there-necked flasks；
4.1gNaOH is weighed, l/10 amounts is first added under agitation, be i.e. 0.41g NaOH, be heated to 80~90 DEG C, exothermic heat of reaction is simultaneously
There are NaCl generations；Maintenance reaction temperature is at 90 DEG C；1/10 amount, i.e. 0.41g NaOH are added after 10min, later every 10min
Add a NaOH, add 1/10, i.e. 0.41g of NaOH total amounts every time, until 4.1gNaOH is added；Continue after reacting 25min
Terminate reaction, obtain reaction solution；At 60-70 DEG C, reacting liquid filtering is removed into accessory substance NaCl, excess is distilled off under decompression
Epoxychloropropane, that is, obtain epoxy resin.
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| CN201610301615.7A CN105820312B (en) | 2016-05-07 | 2016-05-07 | A kind of Chinese medicine dreg prepares the preparation method of epoxy resin |
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| CN201610301615.7A CN105820312B (en) | 2016-05-07 | 2016-05-07 | A kind of Chinese medicine dreg prepares the preparation method of epoxy resin |
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| CN105820312B true CN105820312B (en) | 2018-01-26 |
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2016
- 2016-05-07 CN CN201610301615.7A patent/CN105820312B/en active Active
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| Title |
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| "木质素在环氧树脂合成中的应用进展";冯攀，等;《纤维素科学与技术》;20100630;第18卷(第2期);第54-59页 * |
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| CN105820312A (en) | 2016-08-03 |
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