CN101734648A - Method for preparing water soluble L-cysteine carbon microsphere derivative - Google Patents
Method for preparing water soluble L-cysteine carbon microsphere derivative Download PDFInfo
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- CN101734648A CN101734648A CN200910075860A CN200910075860A CN101734648A CN 101734648 A CN101734648 A CN 101734648A CN 200910075860 A CN200910075860 A CN 200910075860A CN 200910075860 A CN200910075860 A CN 200910075860A CN 101734648 A CN101734648 A CN 101734648A
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Abstract
The invention relates to a method for preparing a water soluble L-cysteine carbon microsphere derivative. The method is characterized by according to the features of the carbon materials and the actual conditions of the externally coated chemical substances, taking acetylene as the carbon source, toluene and ferrocene as the catalysts and argon as the carrier gas to prepare the carbon microsphere at 1000 DEG C in a tube high temperature furnace, preparing the pure carbon microsphere after purifying the carbon microsphere with nitric acid at 100 DEG C, then synthesizing a brownish black externally coated water soluble L-cysteine carbon microsphere derivative with the substances such as L-cysteine hydrochloride in a four-neck flask, and preparing the final product through organic phase and inorganic phase separation, washing, filtration and vacuum drying. The method is advanced, short in process flow and less in used equipment, and the externally coated carbon microsphere derivative has clear appearance, uniform grain size of 400-500nm and stable water solubility and can be matched with various chemical substances to prepare chemical agents, thus being a quite ideal method for preparing the water soluble L-cysteine carbon microsphere derivative.
Description
Technical field
The present invention relates to a kind of preparation method of water soluble L-cysteine carbon microsphere derivative, belong to material derived thing of organic carbon and preparation method's technical field.
Background technology
Carbosphere, it is spherical laminate structure, be the topmost manifestation and the shape characteristic of carbon material, its pattern has solid shape, hollow shape, interior shape, the outsourcing material shape of belonging to covered with gold leaf, its particle diameter has micron order, nano level, can mate with the number of chemical element, makes multiple high value added product, have crucial industrial application value, can be used for high-density high-strength carbon material, catalyzer, gac, lithium ion battery and pharmaceutical raw material etc.
Because carbosphere can only be dissolved in non-polar organic solvent, for example benzene, toluene, hexanaphthene, chloroform, so hindered its application aspect biological chemistry and medical science, therefore studying a kind of water miscible carbon microsphere derivative is crucial academic problem.
Amino acid is to constitute organism the most basic proteinic material, with the vital movement of biology very confidential relation is arranged, and amino acid has L type, D type, the utilization of people's physical efficiency mainly be L type amino acid, the utilization that is absorbed by the body easily of various L type amino acid; The L-halfcystine is the amino acid whose classification of L type, content seldom in general meals, the L-halfcystine can promote conversion, absorption and the utilization of human body internal protein, especially people who drinks beyond one's capacity and liver problem sufferer more need the L-halfcystine, otherwise liver can be subjected to greater loss, research is coated on the carbosphere surface with the covalent linkage form of L-halfcystine, to increase the solubleness of carbosphere in water, synthesize the water-soluble cysteine carbon microsphere derivative that the human liver is had special biological effect, tool has very important significance.
Summary of the invention
Goal of the invention
Purpose of the present invention is exactly the practical situation at background technology, adopt vapour deposition process to prepare carbosphere, and carry out purification process, carry out the synthetic of soluble derivative with the L-cysteine hydrochloride then, make water soluble L-cysteine carbon microsphere derivative, to fill up the scientific research blank of this type of technology.
Technical scheme
The chemical substance material that the present invention uses is: acetylene, ferrocene, argon gas, toluene, deionized water, L-cysteine hydrochloride, dehydrated alcohol, TBAH, hydrogen peroxide, sodium hydroxide, nitric acid, its combination consumption is as follows: with gram, milliliter, centimetre
3Be measure unit
Acetylene: C
2H
210000cm
3± 100cm
3
Ferrocene: Fe (C
5H
5)
24.2g ± 0.1g
Argon gas: Ar 200000cm
3± 100cm
3
L-cysteine hydrochloride: C
3H
7O
2NS 2.0g ± 0.01g
Sodium hydroxide: NaOH 0.85g ± 0.01g
TBAH: C
16H
37NO 1.0ml ± 0.01ml
Toluene: C
6H
5CH
3400ml ± 10ml
Deionized water: H
2O 10000ml ± 100ml
Dehydrated alcohol: CH
3CH
2OH 300ml ± 10ml
Hydrogen peroxide: H
2O
20.5ml ± 0.01ml
Nitric acid: HNO
310ml ± 0.5ml
The preparation method is as follows:
(1) selected chemical substance material
To carry out selectedly to preparing required chemical substance material, and carry out quality purity control:
Acetylene: gaseous state gas 99.5%
Ferrocene: solid-state solid 98.0%
Argon gas: gaseous state gas 99.5%
Toluene: liquid liquid 99.5%
L-cysteine hydrochloride: solid-state solid 99.0%
Sodium hydroxide: solid-state solid 99.5%
TBAH: liquid strength of fluid 20%
Deionized water: liquid liquid 99.5%
Dehydrated alcohol: liquid liquid 99.5%
Nitric acid: liquid strength of fluid 64.5%
(2) preparation carbosphere
1. preparing carbosphere carries out in tube type high-temperature furnace;
2. clean silica tube
Open the silica tube two ends and stop up, carry out the inwall lavation, make its cleaning, dry after the lavation with the 1000ml deionized water;
3. prepare precursor toluene+ferrocene mixing solutions
Take by weighing toluene 40ml ± 0.5ml, ferrocene 4.2g ± 0.1g places beaker, stirs 5min with agitator, stirs the back and becomes: toluene+ferrocene mixing solutions;
4. silica tube is placed middle part in the tube type high-temperature furnace, with plug for seal silica tube two ends, left end inserts acetylene hose, addition funnel, tunger tube, and right-hand member inserts escape pipe;
5. open argon bottle, argon gas valve, tunger tube, in silica tube, import argon gas, drive away obnoxious flavour in the pipe, argon gas input speed 400cm
3/ min;
6. open the addition funnel charging valve, in silica tube, add precursor toluene+ferrocene mixing solutions 3ml;
7. open acetylene cylinder, acetylene valve, acetylene hose, input carbon source in pipe: acetylene gas, acetylene gas input speed 40cm
3/ min;
8. the volume flow ratio of argon gas and acetylene gas is: 10: 1;
9. open escape pipe;
10. open tube type high-temperature furnace, heated quarty tube, temperature begins to heat up by 20 ℃, and heat-up rate is 20 ℃/min, rises to 1000 ℃ ± 5 ℃, at this temperature constant temperature, be incubated, leave standstill 20min ± 1min, makes it carry out chemical reaction, modality, generation product; Chemical equation is as follows:
Behind the chemical reaction, close the tube type high-temperature furnace well heater, close acetylene cylinder, acetylene valve, acetylene hose, under argon shield, make it naturally cool to 20 ℃ ± 3 ℃ with stove;
After 12 coolings, on quartzy tube wall, generate carbosphere product, that is: black carbon microballoon;
Open the silica tube two ends and stop up, with the carbosphere product on the long-armed spoon collection silica tube inwall, standby;
(3) purification process carbosphere
1. black carbon microballoon 0.1g is placed beaker, add nitric acid 10ml ± 0.5ml then, place then on the electric heater, opening electric heater, temperature rises to 100 ℃ ± 2 ℃ by 20 ℃, stirs with agitator then, time 300min ± 10min stirs the back and becomes: the carbosphere salpeter solution;
2. close electric heater, make it naturally cool to 20 ℃ ± 3 ℃;
3. vacuum filtration
The carbosphere salpeter solution is placed on the filter flask, in B, carry out suction filtration with three layers of middling speed qualitative filter paper, retain product on the filter paper: the carbosphere filter cake is nitric acid waste in the filter flask;
4. wash, filter
The carbosphere filter cake is placed beaker, add deionized water 100ml, use the agitator agitator treating, place then on the filter flask, filter, retain the product filter cake on the filter paper with one deck middling speed qualitative filter paper;
Washing, filtration repeat five times;
5. vacuum-drying
The product filter cake is placed quartzy product boat, places vacuum drying oven dry then, 80 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 0.09Pa, time of drying 2160min, after the drying be: the carbosphere powder;
(4) preparation water soluble L-cysteine carbon microsphere derivative
1. prepare toluene+carbosphere mixing solutions
Carbosphere 0.06g behind the purifying, toluene 60ml are placed beaker, stir 10min, become: toluene carbosphere mixing solutions with agitator;
2. prepare L-cysteine hydrochloride+sodium hydroxide+deionized water+dehydrated alcohol quaternary mixing solutions
L-cysteine hydrochloride 2.0g ± 0.01g, sodium hydroxide 0.85g ± 0.01g, deionized water 5ml ± 0.5ml, dehydrated alcohol 40ml ± 1ml are placed beaker, stir 10min, become: the quaternary mixing solutions with agitator;
3. in four-hole boiling flask, be prepared
Insert four dropping funnels successively on four-hole boiling flask top; In four dropping funnels, add respectively:
L-cysteine hydrochloride+sodium hydroxide+deionized water+dehydrated alcohol quaternary mixing solutions 48ml ± 1ml;
Toluene+carbosphere mixing solutions 60ml ± 1ml;
TBAH 1.0ml ± 0.01ml;
Hydrogen peroxide 0.5ml ± 0.01ml;
And drip respectively by above-listed order;
Dropping is carried out under 20 ℃ ± 1 ℃ temperature;
In the dropping process, stir churning time 180min ± 2min with the magnetic agitation ware;
In the dropping process, chemical reaction will take place in each chemical element, and reaction formula is as follows:
In the formula:
In the formula: HOOC: carboxyl
HN: imido grpup
NH
2: amino
COOH: carboxyl
CHCH
2SSCH
2CH: dithio diethyl
Na
2CO
3: yellow soda ash
4. separate organic phase+inorganic phase mixing solutions
Organic phase+inorganic phase mixing solutions is placed the hub trial jar, the hub trial jar is vertically left standstill time 5min ± 0.5min;
After leaving standstill, inorganic phase species precipitate is in the trial jar bottom, and the organic phase material is suspended in trial jar top;
Then with suction pipe with the sucking-off of organic phase material, discard;
Then inorganic phase material is retained in the trial jar;
5. the inorganic phase material of centrifugation is five times
Inorganic phase material in the hub bottle is placed beaker, add dehydrated alcohol 100ml then, stir 5min with agitator;
Place the centrifuge tube of separating centrifuge to carry out centrifugation then, centrifuge speed 5000r/min, centrifugation time 8min, after the centrifugation, top is the dehydrated alcohol waste liquid, discards, the bottom is the black solid material, that is: the L-cysteine carbon microsphere derivative;
Centrifugation repeats five times;
6. deionized water wash, filtration are five times
The black solid material is placed beaker, add deionized water 100ml, with agitator agitator treating 5min;
Place dropping funnel then, filter, retain product filter cake, that is: L-cysteine carbon microsphere derivative product filter cake on the filter paper with two layers of middling speed qualitative filter paper;
Washing, filtration repeat five times;
7. vacuum-drying
The product filter cake is placed quartzy product boat, place vacuum drying oven to carry out vacuum-drying then, drying temperature is 80 ℃ ± 2 ℃, and vacuum tightness is 0.09Pa, and be 2160min time of drying;
After the vacuum-drying, get final product, that is: outer coating, brownish black, water soluble L-cysteine carbon microsphere derivative pressed powder;
(5) detect, chemically examine, analyze, characterize
Pattern, color and luster, composition, the chemical property of water soluble L-cysteine carbon microsphere derivative to preparation detects, chemically examines, analyzes, characterizes;
Carry out X-ray diffraction analysis with Y-2000 type x-ray instrument;
Carry out the exterior appearance analysis with JSM-6700F type awkward silence at a meeting photo-emission electron microscopy;
Carry out the infrared absorption pattern analysis with the FTS-165 infrared spectrometer;
Conclusion: final product is: brownish black, outer coating, water soluble L-cysteine carbon microsphere derivative pressed powder;
Powder diameter is: 400-500nm
(6) store
Brownish black product to preparation is stored in the water white Glass Containers, places cool place, drying, clean environment, waterproof, protection against the tide, sun-proof, acid-proof alkali salt erosion, 20 ℃ ± 3 ℃ of storing temps, relative humidity≤10%.
The preparation of described water soluble L-cysteine carbon microsphere derivative; be to be carbon source with the acetylene gas; with the argon gas is carrier gas and shielding gas; with the ferrocene is catalyzer; with toluene is solvent; with nitric acid is carbosphere solvent and purifying agent; with the L-cysteine hydrochloride is the water-soluble coating of carbosphere; with the TBAH is consisting of phase-transferring agent; with the hydrogen peroxide is oxygenant; with the dehydrated alcohol is the precipitating agent, is clean-out system, washing composition and solvating agent with the deionized water, is acidity-basicity regulator with sodium hydroxide.
The water soluble L-cysteine carbon microsphere derivative pattern of described preparation is: brownish black, coat pressed powder outward, powder diameter is 400-500nm.
Beneficial effect
The present invention compares with background technology has tangible advance; it is the characteristic according to carbon material; the outer practical situation that coat chemical substance; with acetylene is carbon source; with toluene+ferrocene is catalyzer; with the argon gas is carrier gas and shielding gas; in tube type high-temperature furnace, under 1000 ℃ of states, make carbosphere; make the purified carbon microballoon through nitric acid purifying under 100 ℃ of states; in four-hole boiling flask, synthesize brownish black then with materials such as L-cysteine hydrochlorides; the outer coating; water soluble L-cysteine carbon microsphere derivative; through organic phase; inorganic being separated; washing; filter and vacuum-drying; make final product; this preparation method advanced person; technical process is short; use equipment is few; the outer carbon microsphere derivative pattern that coats is clear; particle diameter is even; there is not agglomeration; has stable water soluble characteristic; can make chemical agent with number of chemical material coupling, be the very good method for preparing water soluble L-cysteine carbon microsphere derivative.
Description of drawings
Fig. 1 prepares the carbosphere state graph for tube type high-temperature furnace
Fig. 2 is tube type high-temperature furnace Heating temperature and time coordinate graph of a relation
Fig. 3 is carbosphere nitric acid purified state figure
Fig. 4 is the state graph of four-hole boiling flask synthesizing water-solubility L-cysteine carbon microsphere derivative
Fig. 5 is a water soluble L-cysteine carbon microsphere derivative product shape appearance figure
Fig. 6 is a water soluble L-cysteine carbon microsphere derivative product diffracted intensity collection of illustrative plates
Fig. 7 is the water soluble L-cysteine carbon microsphere derivative infrared absorpting light spectra
Shown in the figure, list of numerals is as follows:
1, High Temperature Furnaces Heating Apparatus, 2, silica tube, 3, escape pipe, 4, stop up; 5, track, 6, the stove seat, 7, argon bottle, 8, tunger tube, 9, the argon gas valve, 10, liquid adding bottle, 11, charging valve, 12, addition funnel, 13, the acetylene valve, 14, acetylene cylinder, 15, acetylene hose, 16, agitator, 17, nitric acid+carbosphere solution, 18, beaker, 19, well heater, 20, dropping funnel, 21, the quaternary mixing solutions, 22, dropping funnel, 23, hydrogen peroxide, 24, dropping funnel, 25, toluene+carbosphere, 26, dropping funnel, 27, TBAH, 28, stir ware, 29, resulting solution, 30, stop up 31, four-hole boiling flask, 32, carbosphere.
Embodiment
The present invention will be further described below in conjunction with accompanying drawing:
Shown in Figure 1; for tube type high-temperature furnace prepares the carbosphere state graph; it is correct that want each position, and obstruction will be blocked up the jail, will seal in the pipe; escape pipe is unobstructed; acetylene and argon flow amount volume ratio are 1: 10, and the toluene+ferrocene in the addition funnel wants flow velocity moderate, High Temperature Furnaces Heating Apparatus heat temperature raising to 1000 ℃; increase progressively with the heat-up rate of 20 ℃/min and to carry out, the preparation back naturally cools to 20 ℃ under argon shield.
In the High Temperature Furnaces Heating Apparatus 1 is silica tube 2, silica tube is contained on the track 5, silica tube 2 left parts are provided with and stop up 30, stop up 30 and are provided with liquid adding bottle 10, charging valve 11, addition funnel 12, acetylene hose 15, acetylene valve 13, acetylene cylinder 14, tunger tube 8, argon gas valve 9, argon bottle 7, and High Temperature Furnaces Heating Apparatus places on the stove seat 6.
Shown in Figure 2, be tube type high-temperature furnace Heating temperature and time coordinate graph of a relation, temperature begins to heat up by 20 ℃, i.e. 80 ℃/min of A point heat-up rate, rise to 1000 ℃, promptly the B point is incubated 20min at this temperature constant temperature, be the B-C section, naturally cool to 20 ℃ then, be i.e. the D point.
Shown in Figure 3, be carbosphere nitric acid purified state figure, in beaker, carry out for 100 ℃, evenly stir in temperature, on electric heater 13, be beaker 18, establish agitator 16 in the beaker, be nitric acid+carbosphere solution in the beaker.
Shown in Figure 4, be water soluble L-cysteine carbon microsphere derivative synthetic state figure, under 20 ℃ ± 1 ℃, drip four kinds of mixing solutionss respectively, stir through agitator, make organic phase+inorganic phase mixed solution; On agitator 28 tops is four-hole boiling flask 31, four-hole boiling flask 31 tops are provided with dropping funnel 20,22,24,26, being respectively quaternary mixing solutions 21, hydrogen peroxide 23, toluene+carbosphere 25, TBAH 27 in it, is resulting solution 29 in the four-hole boiling flask 31.
Shown in Figure 5, be the final product shape appearance figure, among the figure as can be known: the product pattern is the brownish black particulate state, is irregular stacking, and uniform particles does not have agglomeration.
Shown in Figure 6, be final product diffracted intensity collection of illustrative plates, ordinate zou is the diffracted intensity index, X-coordinate is diffraction angle 2 θ, has occurred the diffraction peak of C (002) near 2 θ=25 °, shows that product has good degree of graphitization.
Shown in Figure 7, be the final product infrared spectrogram, as can be known, wave number is 3463.2cm among the figure
-1What the place was corresponding is N-H stretching vibration absorption peak, and wave number is 3030.7cm
-1Near corresponding be O-H stretching vibration peak, wave number is 1585.2cm
-1The absorption peak that the place occurs is ionization-COO-vibration peak, show and added various water miscible functional groups in the product, need to prove, the infrared absorption spectrum of product is not the simple superposition of carbosphere and L-cysteine hydrochloride infrared absorption spectrum, but under the interaction between carbosphere and the L-halfcystine between the two charge transfer is taking place, the INFRARED SPECTRUM of carbosphere red shift occurred and has formed.
Preparation principle is as follows:
Carbon atom in the carbosphere can be from-1 valency gradual deoxidizing to-6 valencys, many different types of nucleophilic reagents all can with the carbon atom generation addition reaction in the carbosphere, the nitrogen of ammonium class contains unpaired electron, very strong nucleophilie nucleus ability is arranged, it also can with carbon atom generation addition reaction, the L-halfcystine have dual-functional group because of, it also has amino except that carboxyl, the L-halfcystine can generate 1, the 2-adduct with the carbon atom in the carbosphere; Reaction according to this principle supposition carbosphere and L-halfcystine can be thought following process: the first step is to form cysteine salt, second step was to form the amino nitrogen free radical, it can form by the direct transfer of H, has proved that carbon atom can generate singlet state O very effectively
2, and singlet state O
2Can catch the H atom, find in the experiment, a small amount of O
2Existence reaction is had booster action, in addition, this free radical also can form by electron-transfer reaction and proton dissociation subsequently, the 3rd step was that free radical addition is to two keys of carbosphere, open the two keys of 1 C-C, obtain hydrogen, finally form stable carbon microsphere derivative.
Claims (3)
1. the preparation method of a water soluble L-cysteine carbon microsphere derivative, it is characterized in that: the chemical substance material of use is: acetylene, ferrocene, argon gas, toluene, deionized water, L-cysteine hydrochloride, dehydrated alcohol, TBAH, hydrogen peroxide, sodium hydroxide, nitric acid, its combination consumption is as follows: with gram, milliliter, centimetre
3Be measure unit
Acetylene: C
2H
210000cm
3± 100cm
3
Ferrocene: Fe (C
5H
5)
24.2g ± 0.1g
Argon gas: Ar 200000cm
3± 100cm
3
L-cysteine hydrochloride: C
3H
7O
2NS 2.0g ± 0.01g
Sodium hydroxide: NaOH 0.85g ± 0.01g
TBAH: C
16H
37NO 1.0ml ± 0.01ml
Toluene: C
6H
5CH
3400ml ± 10ml
Deionized water: H
2O 10000ml ± 100ml
Dehydrated alcohol: CH
3CH
2OH 300ml ± 10ml
Hydrogen peroxide: H
2O
20.5ml ± 0.01ml
Nitric acid: HNO
310ml ± 0.5ml
The preparation method is as follows:
(1) selected chemical substance material
To carry out selectedly to preparing required chemical substance material, and carry out quality purity control:
Acetylene: gaseous state gas 99.5%
Ferrocene: solid-state solid 98.0%
Argon gas: gaseous state gas 99.5%
Toluene: liquid liquid 99.5%
L-cysteine hydrochloride: solid-state solid 99.0%
Sodium hydroxide: solid-state solid 99.5%
TBAH: liquid strength of fluid 20%
Deionized water: liquid liquid 99.5%
Dehydrated alcohol: liquid liquid 99.5%
Nitric acid: liquid strength of fluid 64.5%
(1) preparation carbosphere
1. preparing carbosphere carries out in tube type high-temperature furnace;
2. clean silica tube
Open the silica tube two ends and stop up, carry out the inwall lavation, make its cleaning, dry after the lavation with the 1000ml deionized water;
3. prepare precursor toluene+ferrocene mixing solutions
Take by weighing toluene 40ml ± 0.5ml, ferrocene 4.2g ± 0.1g places beaker, stirs 5min with agitator, stirs the back and becomes: toluene+ferrocene mixing solutions;
4. silica tube is placed middle part in the tube type high-temperature furnace, with plug for seal silica tube two ends, left end inserts acetylene hose, addition funnel, tunger tube, and right-hand member inserts escape pipe;
5. open argon bottle, argon gas valve, tunger tube, in silica tube, import argon gas, drive away obnoxious flavour in the pipe, argon gas input speed 400cm
3/ min;
6. open the addition funnel charging valve, in silica tube, add precursor toluene+ferrocene mixing solutions 3ml;
7. open acetylene cylinder, acetylene valve, acetylene hose, input carbon source in pipe: acetylene gas, acetylene gas input speed 40cm
3/ min;
8. the volume flow ratio of argon gas and acetylene gas is: 10: 1;
9. open escape pipe;
10. open tube type high-temperature furnace, heated quarty tube, temperature begins to heat up by 20 ℃, and heat-up rate is 20 ℃/min, rises to 1000 ℃ ± 5 ℃, at this temperature constant temperature, be incubated, leave standstill 20min ± 1min, makes it carry out chemical reaction, modality, generation product;
Chemical equation is as follows:
Behind the chemical reaction, close the tube type high-temperature furnace well heater, close acetylene cylinder, acetylene valve, acetylene hose, under argon shield, make it naturally cool to 20 ℃ ± 3 ℃ with stove;
(3) purification process carbosphere
1. black carbon microballoon 0.1g is placed beaker, add nitric acid 10ml ± 0.5ml then, place then on the electric heater, opening electric heater, temperature rises to 100 ℃ ± 2 ℃ by 20 ℃, stirs with agitator then, time 300min ± 10min stirs the back and becomes: the carbosphere salpeter solution;
2. close electric heater, make it naturally cool to 20 ℃ ± 3 ℃;
3. vacuum filtration
The carbosphere salpeter solution is placed on the filter flask, in B, carry out suction filtration with three layers of middling speed qualitative filter paper, retain product on the filter paper: the carbosphere filter cake is nitric acid waste in the filter flask;
4. wash, filter
The carbosphere filter cake is placed beaker, add deionized water 100ml, use the agitator agitator treating, place then on the filter flask, filter, retain the product filter cake on the filter paper with one deck middling speed qualitative filter paper;
Washing, filtration repeat five times;
5. vacuum-drying
The product filter cake is placed quartzy product boat, places vacuum drying oven dry then, 80 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 0.09Pa, time of drying 2160min, after the drying be: the carbosphere powder;
(4) preparation water soluble L-cysteine carbon microsphere derivative
1. prepare toluene+carbosphere mixing solutions
Carbosphere 0.06g behind the purifying, toluene 60ml are placed beaker, stir 10min, become: toluene carbosphere mixing solutions with agitator;
2. prepare L-cysteine hydrochloride+sodium hydroxide+deionized water+dehydrated alcohol quaternary mixing solutions
L-cysteine hydrochloride 2.0g ± 0.01g, sodium hydroxide 0.85g ± 0.01g, deionized water 5ml ± 0.5ml, dehydrated alcohol 40ml ± 1ml are placed beaker, stir 10min, become: the quaternary mixing solutions with agitator;
3. in four-hole boiling flask, be prepared
Insert four dropping funnels successively on four-hole boiling flask top; In four dropping funnels, add respectively:
L-cysteine hydrochloride+sodium hydroxide+deionized water+dehydrated alcohol quaternary mixing solutions 48ml ± 1ml;
Toluene+carbosphere mixing solutions 60ml ± 1ml;
TBAH 1.0ml ± 0.01ml;
Hydrogen peroxide 0.5ml ± 0.01ml;
And drip respectively by above-listed order;
Dropping is carried out under 20 ℃ ± 1 ℃ temperature;
In the dropping process, stir churning time 180min ± 2min with the magnetic agitation ware;
In the dropping process, chemical reaction will take place in each chemical element, and reaction formula is as follows:
In the formula:
In the formula: HOOC: carboxyl
HN: imido grpup
NH
2: amino
COOH: carboxyl
CHCH
2SSCH
2CH: dithio diethyl
Na
2CO
3: yellow soda ash
4. separate organic phase+inorganic phase mixing solutions
Organic phase ten inorganic phase mixing solutionss are placed the hub trial jar, the hub trial jar is vertically left standstill time 5min ± 0.5min;
After leaving standstill, inorganic phase species precipitate is in the trial jar bottom, and the organic phase material is suspended in trial jar top;
Then with suction pipe with the sucking-off of organic phase material, discard;
Then inorganic phase material is retained in the trial jar;
5. the inorganic phase material of centrifugation is five times
Inorganic phase material in the hub bottle is placed beaker, add dehydrated alcohol 100ml then, stir 5min with agitator;
Place the centrifuge tube of separating centrifuge to carry out centrifugation then, centrifuge speed 5000r/min, centrifugation time 8min, after the centrifugation, top is the dehydrated alcohol waste liquid, discards, the bottom is the black solid material, that is: the L-cysteine carbon microsphere derivative;
Centrifugation repeats five times;
6. deionized water wash, filtration are five times
The black solid material is placed beaker, add deionized water 100ml, with agitator agitator treating 5min;
Place dropping funnel then, filter, retain product filter cake, that is: L-cysteine carbon microsphere derivative product filter cake on the filter paper with two layers of middling speed qualitative filter paper;
Washing, filtration repeat five times;
7. vacuum-drying
The product filter cake is placed quartzy product boat, place vacuum drying oven to carry out vacuum-drying then, drying temperature is 80 ℃ ± 2 ℃, and vacuum tightness is 0.09Pa, and be 2160min time of drying;
After the vacuum-drying, get final product, that is: outer coating, brownish black, water soluble L-cysteine carbon microsphere derivative pressed powder;
(5) detect, chemically examine, analyze, characterize
Pattern, color and luster, composition, the chemical property of water soluble L-cysteine carbon microsphere derivative to preparation detects, chemically examines, analyzes, characterizes;
Carry out X-ray diffraction analysis with Y-2000 type x-ray instrument;
Carry out the exterior appearance analysis with JSM-6700F type awkward silence at a meeting photo-emission electron microscopy;
Carry out the infrared absorption pattern analysis with the FTS-165 infrared spectrometer;
Conclusion: final product is: brownish black, outer coating, water soluble L-cysteine carbon microsphere derivative pressed powder;
Powder diameter is: 400-500nm
(6) store
Brownish black product to preparation is stored in the water white Glass Containers, places cool place, drying, clean environment, waterproof, protection against the tide, sun-proof, acid-proof alkali salt erosion, 20 ℃ ± 3 ℃ of storing temps, relative humidity≤10%.
2. according to the preparation method of claims 1 described a kind of water soluble L-cysteine carbon microsphere derivative; it is characterized in that: the preparation of described water soluble L-cysteine carbon microsphere derivative; be to be carbon source with the acetylene gas; with the argon gas is carrier gas and shielding gas; with the ferrocene is catalyzer; with toluene is solvent; with nitric acid is carbosphere solvent and purifying agent; with the L-cysteine hydrochloride is the water-soluble coating of carbosphere; with the TBAH is consisting of phase-transferring agent, is oxygenant with the hydrogen peroxide, is the precipitating agent with the dehydrated alcohol; with the deionized water is clean-out system; washing composition and solvating agent are acidity-basicity regulator with sodium hydroxide.
3. according to the preparation method of claims 1 described a kind of water soluble L-cysteine carbon microsphere derivative, it is characterized in that: the water soluble L-cysteine carbon microsphere derivative pattern of described preparation is: brownish black, coat pressed powder outward, powder diameter is 400-500nm.
Priority Applications (1)
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|---|---|---|---|
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| CN113831259B (en) * | 2021-11-05 | 2023-07-25 | 内蒙古工业大学 | Synthesis method of aromatic azo compound |
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