CN110483595A - A kind of process for refining of medicinal grade cane sugar - Google Patents
A kind of process for refining of medicinal grade cane sugar Download PDFInfo
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- CN110483595A CN110483595A CN201910827026.6A CN201910827026A CN110483595A CN 110483595 A CN110483595 A CN 110483595A CN 201910827026 A CN201910827026 A CN 201910827026A CN 110483595 A CN110483595 A CN 110483595A
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- cane sugar
- ethanol solution
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- grade cane
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- 229930006000 Sucrose Natural products 0.000 title claims abstract description 142
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 title claims abstract description 141
- 229960004793 sucrose Drugs 0.000 title claims abstract description 140
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000007670 refining Methods 0.000 title claims abstract description 22
- 230000008569 process Effects 0.000 title claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 132
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 118
- 239000005720 sucrose Substances 0.000 claims abstract description 62
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 57
- 238000001179 sorption measurement Methods 0.000 claims abstract description 47
- 239000000463 material Substances 0.000 claims abstract description 34
- 230000007935 neutral effect Effects 0.000 claims abstract description 27
- 239000000706 filtrate Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 239000000779 smoke Substances 0.000 claims abstract description 21
- 239000012141 concentrate Substances 0.000 claims abstract description 11
- 238000001953 recrystallisation Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000002425 crystallisation Methods 0.000 claims abstract description 10
- 230000008025 crystallization Effects 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000005119 centrifugation Methods 0.000 claims abstract description 4
- 238000010298 pulverizing process Methods 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims abstract description 4
- 235000019441 ethanol Nutrition 0.000 claims 7
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 229960004756 ethanol Drugs 0.000 description 43
- 238000010521 absorption reaction Methods 0.000 description 13
- 238000005516 engineering process Methods 0.000 description 13
- 230000009467 reduction Effects 0.000 description 13
- 239000003610 charcoal Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 11
- 229960000935 dehydrated alcohol Drugs 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 239000003814 drug Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 230000007423 decrease Effects 0.000 description 7
- 229940079593 drug Drugs 0.000 description 6
- 235000021552 granulated sugar Nutrition 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 159000000007 calcium salts Chemical class 0.000 description 5
- 238000004040 coloring Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 238000011835 investigation Methods 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 238000012216 screening Methods 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- 238000011020 pilot scale process Methods 0.000 description 4
- 235000000346 sugar Nutrition 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical group C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000000274 adsorptive effect Effects 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 150000008442 polyphenolic compounds Chemical class 0.000 description 2
- 235000013824 polyphenols Nutrition 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001223 reverse osmosis Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 206010019233 Headaches Diseases 0.000 description 1
- 102000001554 Hemoglobins Human genes 0.000 description 1
- 108010054147 Hemoglobins Proteins 0.000 description 1
- 240000000111 Saccharum officinarum Species 0.000 description 1
- 235000007201 Saccharum officinarum Nutrition 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 230000003260 anti-sepsis Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000001684 chronic effect Effects 0.000 description 1
- 231100000762 chronic effect Toxicity 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 210000003743 erythrocyte Anatomy 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/04—Disaccharides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention provides a kind of process for refining of medicinal grade cane sugar, including Step 1: 1.5 ~ 3 times of sucrose material weight of ethanol solution is added in a kettle, the neutral alcohol solution that ethanol solution is 40 ~ 90%, is heated to 40 ~ 85 DEG C for neutral alcohol solution, neutral hot ethanol solution is made；Step 2: the active carbon of sucrose material and sucrose material quality 0.2 ~ 1.0% is added in neutral hot ethanol solution, activated carbon adsorption reaction is carried out, 40 ~ 85 DEG C keep the temperature and stir 5 ~ 60min, and it is cooling, obtain primary first-order equation liquid；Active carbon is removed Step 3: primary first-order equation liquid is filtered, obtains smoke filtrate；Step 4: smoke filtrate is concentrated into 1.2 ~ 1.5 times of sucrose material weight, concentrate is obtained；Step 5: crystallization is collected in recrystallization, centrifugation；Step 6: pulverizing and sieving after crystallizing and drying, medicinal grade cane sugar is obtained.The medicinal grade cane sugar refined through the present invention has the advantages that at low cost, batch production, quality are high.
Description
Technical field
The present invention relates to pharmaceutical chemistry technical field more particularly to a kind of process for refining of medicinal grade cane sugar.
Background technique
Recent domestic is increasingly stringenter the quality criteria requirements of preparation in terms of pharmaceutical drugs and medicine management, doctor
Medicine grade cane sugar due to purity is high, impurity it is few, can replace food grade sucrose be used as pharmaceutic adjuvant, can ensure drug quality with
Drug safety.
With State Food and Drug Administration to Chinese Pharmacopoeia strictly implement and execute development produce it is medicinal
Grade cane sugar is for guaranteeing that drug safety is of great significance.Sucrose mostly uses sulfurous method to produce greatly, so that in Sucrose products also
There are the toxic heavy metals such as a large amount of sulphite and a certain amount of arsenic, lead, the sulphite in sucrose has reproducibility, display drift
White, decoloration, anti-oxidant and antisepsis, sulphite toxicity is smaller, and when people takes on a small quantity, rapid oxidation is at sulfuric acid in vivo
Salt excretes, and Chronic Effect can cause to have a headache, and has certain damage to liver, reduces erythrocyte hemoglobin.
Currently, the refining methd of sucrose is macroporous absorbent resin absorption method, ion exchange resin exchange process, flocculant precipitating
Method, reverse osmosis membrane filtration method and recrystallization method etc..Macroporous absorbent resin absorption method and ion exchange resin exchange process are in purification sugarcane
The processing suitable for small lot of sugar, the cost of resin is relatively high, and can generate a large amount of discharging of waste liquid, causes environmental pollution；
The long processing period of the flocculant precipitation method will cause the conversion of sucrose, influence the purity and yield of sucrose；Reverse osmosis membrane filtration method
There is also the small problems of equipment cost height, treating capacity.
In view of this, it is necessary to the process for refining of sucrose in the prior art be improved, to solve the above problems.
Summary of the invention
It is an object of the invention to solve the problems, such as at high cost, low efficiency in sucrose subtractive process, not can manufacture, mention
A kind of process for refining of medicinal grade cane sugar is gone out.The medical grade cane sugar of purification is for common sucrose in color, sulfate
Content, concentration of metal ions etc. all have biggish raising, can satisfy the regulation of the medicinal grade cane sugar of national standard.
Realize that the technical solution of goal of the invention is as follows: a kind of process for refining of medicinal grade cane sugar, comprising the following steps:
Step 1: 1.5~3 times of sucrose material weight of ethanol solution is added in a kettle, ethanol solution is 40~
Neutral alcohol solution is heated to 40~85 DEG C by 90% neutral alcohol solution, and neutral hot ethanol solution is made；
Step 2: the active carbon of sucrose material and sucrose material quality 0.2~1.0% is added in neutral hot ethanol solution,
Activated carbon adsorption reaction is carried out, 40~85 DEG C keep the temperature and stir 5~60min, and it is cooling, obtain primary first-order equation liquid；
Active carbon is removed Step 3: primary first-order equation liquid is filtered, obtains smoke filtrate；
Step 4: smoke filtrate is concentrated into 1.2~1.5 times of sucrose material weight, concentrate is obtained；
Step 5: crystallization is collected in recrystallization, centrifugation；
Step 6: pulverizing and sieving after crystallizing and drying, medicinal grade cane sugar is obtained.
The purification principle of the medicinal grade cane sugar of the present invention is: using active carbon absorption technology and ethanol solution recrystallizing technology pair
Sucrose material is refined.
Active carbon absorption technology is used to remove the coloring matter and a small amount of nonsugar in sucrose material, reaction mechanism
It is: on the one hand, using the absorption principle of active carbon, in decolorization, is not only able to remove coloring matter, additionally it is possible to absorption ash
Point, organic non-sugar and inorganic salts etc.；On the other hand, active carbon has the structure of fragrant ring type, can be adsorbed and removed sucrose
Aromatic series organic matter in raw material, and since the pigment in sucrose material is mainly polyphenols, active carbon can be removed preferably
Remove polyphenols.Therefore, it can be ensured through medicinal grade cane sugar quality and yield made from active carbon absorption technology.
Ethanol solution recrystallizing technology is mainly used for that treated obtains primary first-order equation liquid by active carbon absorption technology, presses
After certain volume concentration, crystalline patent medicine is crystallized with grade cane sugar, so that medicinal grade cane sugar is made, residue on ignition, calcium salt, sulfuric acid
Salt, solution colour etc. can reach quality standards.
For medicinal grade cane sugar in subtractive process, conductivity is an important technology index of sucrose sublimate degree, is needed tight
Lattice control, currently, the conductivity of medicinal grade cane sugar need to control below 35 μ s/cm.
As a further refinement of the present invention, in step 2, experiment proves that, it is medicinal with the increase of amounts of activated carbon
Grade cane sugar conductivity decreases.When active carbon additional amount is 0.2~0.3%, medicinal grade cane sugar conductivity is greater than 35 μ s/
cm；When active carbon additional amount is 0.3~0.6%, medicinal grade cane sugar conductivity reduction amplitude is big, more obviously；Work as active carbon
When additional amount is 0.6~1.0%, medicinal grade cane sugar conductivity reduction amplitude is slow, and conductivity tends towards stability.It is raw for strict control
Cost is produced, and convenient for filtering to primary first-order equation liquid, active carbon additional amount is the 0.6~0.8% of sucrose material.
As a further refinement of the present invention, in step 1, experiment proves that, with the increase of ethanol solution concentration,
Medicinal grade cane sugar conductivity decreases, and for ethanol solution concentration at 40~50%, medicinal grade cane sugar conductivity reduction amplitude is big,
It is more obvious.When ethanol solution concentration is 50~90%, medicinal grade cane sugar conductivity reduction amplitude is slow, tends towards stability.For
Control production supplementary material cost, and convenient for the suction filtration of primary first-order equation liquid, ethanol solution concentration is 50~80%.
As a further refinement of the present invention, in step 2, experiment proves that, with activated carbon adsorption reaction temperature
It increases, medicinal grade cane sugar conductivity decreases.In general, the viscosity of sucrose is high when adsorption temp is lower, activated carbon adsorption
Ability is big, but the adsorption rate of active carbon is slack-off.When adsorption temp increases, the viscosity of sucrose is reduced, the diffusion of coloring matter
Speed is accelerated, and is easy to adhere in activated carbon surface and its internal capillary, the adsorption rate of active carbon becomes faster.And work as activated carbon adsorption
When temperature is 40~50 DEG C, it is big and obvious that medicinal grade cane sugar conductivity reduces amplitude.Continue to increase with adsorption temp, with grade
Sucrose conductivity reduction amplitude, which becomes smaller, to slow down.And with the raising of activated carbon adsorption reaction temperature, the conversion rate of sucrose increases,
Therefore, to ensure the conductivity of medicinal grade cane sugar, to the control of production cost, the conversion for avoiding sucrose excessive, activated carbon adsorption
The temperature of reaction is 50~70 DEG C.
Experiment proves that medicinal grade cane sugar conductivity decreases with the increase in activated carbon adsorption reaction time.Work as work
Property charcoal be added within initial 25 minutes, it is big and obvious that medicinal grade cane sugar conductivity reduces amplitude, as activated carbon adsorption is reacted
Time continues to extend, and close to saturation, medicinal grade cane sugar conductivity reduction amplitude becomes smaller to slow down activated carbon adsorptive capacity.To improve
Production efficiency controls production cost, and the activated carbon adsorption reaction time is 25~35min.
As a further refinement of the present invention, in step 4, when sucrose recrystallization, volume is smaller after concentration, sucrose knot
Crystalline substance amount is more, but the precipitations such as sulfate, calcium salt become more therewith, influence the quality of medicinal grade cane sugar.Crystallization darkens, and influences medicine
With the color of grade cane sugar.Therefore, the volume of concentrate is 1.3~1.4 times of sucrose material weight when recrystallization, and smoke filtrate is dense
The temperature of contracting is 40~50 DEG C.
Compared with prior art, the invention has the advantage that: the process for refining of medicinal grade cane sugar of the invention, work
Skill is simple, and production cost is low, can be realized batch production.Medicinal grade cane sugar through process for refining preparation is odorless, tasteless white
Color powder, yield are 80.0~90.0%, and the indexs such as sulfate, reduced sugar, residue on ignition, calcium salt, heavy metal meet
The regulation of national standard medical cane sugar.
Detailed description of the invention
Fig. 1 is the flow chart of the medicinal grade cane sugar process for refining of the present invention；
Fig. 2 be in the present invention in active carbon absorption technology after different activities charcoal additional amount medicinal grade cane sugar conductivity variations
Curve graph；
Fig. 3 be in the present invention in active carbon absorption technology after different ethanol solution concentrations medicinal grade cane sugar conductivity variations
Curve graph；
Fig. 4 is that the conductivity of medicinal grade cane sugar becomes after different activities charcoal adsorption time in active carbon absorption technology in the present invention
Change curve graph；
Fig. 5 is that the conductivity of medicinal grade cane sugar becomes after different activities charcoal adsorption temp in active carbon absorption technology in the present invention
Change curve graph；
Fig. 6 is the conductivity variations curve of medicinal grade cane sugar after recrystallizing concentration volume in the present invention in recrystallizing technology
Figure.
Specific embodiment
Invention is described in detail in each embodiment shown in reference to the accompanying drawing, but it should be stated that, these realities
The mode of applying not is limitation of the present invention, those of ordinary skill in the art according to these embodiments made by function, method or
Equivalent transformation or substitution in person's structure, all belong to the scope of protection of the present invention within.
In the description of the present embodiment, it is to be understood that term " center ", " longitudinal direction ", " transverse direction ", "upper", "lower",
The orientation or positional relationship of the instructions such as "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outside" is
It is based on the orientation or positional relationship shown in the drawings, is merely for convenience of description the invention and simplifies description, rather than indicate
Or imply that signified device or element must have a particular orientation, be constructed and operated in a specific orientation, therefore cannot understand
For the limitation to the invention.
In addition, term " first ", " second ", " third " etc. are used for description purposes only, it is not understood to indicate or imply
Relative importance or the quantity for implicitly indicating indicated technical characteristic.The feature of " first ", " second " etc. is defined as a result,
It can explicitly or implicitly include one or more of the features.In the description of the invention, unless otherwise indicated,
The meaning of " plurality " is two or more.
Term " installation ", " connected ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, be also possible to removable
Connection is unloaded, or is integrally connected；It can be mechanical connection, be also possible to be electrically connected；It can be directly connected, it can also be in
Between medium be indirectly connected, can be the connection inside two elements.For the ordinary skill in the art, can pass through
Concrete condition understands concrete meaning of the above-mentioned term in the invention.
Embodiment 1:
A kind of process for refining of medicinal grade cane sugar, as shown in Figure 1, comprising the following steps:
Step 1: 1.5~3 times of sucrose material weight of ethanol solution is added in a kettle, ethanol solution is 40~
Neutral alcohol solution is heated to 40~85 DEG C by 95% neutral alcohol solution, and neutral hot ethanol solution is made；
Step 2: the active carbon of sucrose material and sucrose material quality 0.3~1.0% is added in neutral hot ethanol solution,
Activated carbon adsorption reaction is carried out, 40~85 DEG C keep the temperature and stir 5~60min, and it is cooling, obtain primary first-order equation liquid；
Active carbon is removed Step 3: primary first-order equation liquid is filtered, obtains smoke filtrate；
Step 4: smoke filtrate is concentrated into 1.2~1.5 times of sucrose material weight, concentrate is obtained；
Step 5: crystallization is collected in recrystallization, centrifugation；
Step 6: pulverizing and sieving after crystallizing and drying, medicinal grade cane sugar is obtained.
Embodiment 2:
The present embodiment is the optimal screening of parameters in the process for refining of medicinal grade cane sugar in embodiment 1.
Sucrose conductance measurement method are as follows: the deionized water configuration 85% of 9ml is added in 95% dehydrated alcohol for taking 74ml
Ethanol solution.Every part of configuration 85% of ethanol solution is heated to 80 DEG C, 50g white granulated sugar is added, is stirred at a temperature of 80 DEG C
It mixes 30 minutes, filters, remove active carbon, filtrate measures conductivity.
The present invention is measured using the conductivity meter of upper Haikang instrument Instrument Ltd., the Conductivity Calculation method of sucrose
Are as follows:
Wherein, the conductivity of sample is measured when CT is T DEG C
K is the value of standard KCl solution (i.e. 0.0025mol/L) at T DEG C；
S is standard KCl solution (i.e. 0.0025mol/L) measured value at T DEG C；
C20The conductivity for being sample at 20 DEG C.
For the ethanol solution concentration of active carbon absorption technology, sorption reaction time, active carbon additional amount, adsorption temp etc.
Single factor experiment is carried out, determines optimal technological parameter.
1. the screening of active carbon additional amount:
95% dehydrated alcohol for taking 74ml is added the ethanol solution of the deionized water configuration 85% of 9ml, configures 9 parts altogether.
Every part of configuration 85% of ethanol solution is heated to 80 DEG C, is added 50g white granulated sugar, then by White Sugar Quality 0.2%,
0.3%, 0.4% ..., 0.9%, 1.0% active carbon is added in 1~No. 9 test, and 30 points are stirred at a temperature of 80 DEG C
Clock, filtering remove active carbon, and filtrate measures conductivity, the results are shown in Table one:
Table one: the investigation of different activities charcoal additional amount
Analysis: charted according to data in above table, as shown in Fig. 2, by Fig. 2 it is found that with amounts of activated carbon increase,
Medicinal grade cane sugar conductivity decreases.When active carbon additional amount is 0.2~0.3%, medicinal grade cane sugar conductivity is greater than 35 μ
s/cm；When active carbon additional amount is 0.3~0.6%, medicinal grade cane sugar conductivity reduction amplitude is big, more obviously；Work as activity
When charcoal additional amount is 0.6~1.0%, medicinal grade cane sugar conductivity reduction amplitude is slow, and conductivity tends towards stability.For strict control
Production cost, and convenient for being filtered to primary first-order equation liquid, and prevent excessive active carbon use from causing environmental pollution, activity
Charcoal additional amount is the 0.6~0.8% of sucrose material.
2. the screening of ethanol solution concentration:
Use 95% dehydrated alcohol configuration concentration for 30%, 40%, 50%, 60%, 70%, 80%, 90%.Take 85ml
The ethanol solution of configuration is heated to 80 DEG C, is separately added into 50g white granulated sugar and 0.5g active carbon, and 30 points are stirred at a temperature of 80 DEG C
Clock, filtering remove active carbon, and filtrate measures conductivity, the results are shown in Table two:
Table two: different ethanol concentration is investigated
Analysis: ethanol solution can accelerate activated carbon adsorption coloring matter as a kind of organic polar solvent, according to above-mentioned table
Data are charted in lattice, as shown in figure 3, by Fig. 3 it is found that as ethanol solution concentration increases, the continuous drop of the conductivity of sucrose
It is low.For ethanol solution concentration at 40~50%, medicinal grade cane sugar conductivity reduction amplitude is big, more obviously.When ethanol solution is dense
For degree at 50~90%, medicinal grade cane sugar conductivity reduction amplitude is slow, tends towards stability.Supplementary material cost is produced for control, with
And the suction filtration convenient for primary first-order equation liquid, ethanol solution concentration are 50~80%.
3. the screening of activated carbon adsorption temperature:
95% dehydrated alcohol for taking 43ml is added the ethanol solution of the deionized water configuration 55% of 40ml, configures 7 altogether
Part.Ethanol solution is separately heated to 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, be separately added into 50g white granulated sugar and
0.5g active carbon keeps the temperature and stirs 30 minutes, filtering, removes active carbon, and filtrate measures conductivity, the results are shown in Table three:
Table three: the investigation of different activities charcoal adsorption temp
Analysis, charted according to data in above table, as shown in figure 4, by Fig. 4 it is found that as activated carbon adsorption is reacted
The raising of temperature, medicinal grade cane sugar conductivity decrease.In general, the viscosity of sucrose is high when adsorption temp is lower, activity
Charcoal adsorption capacity is big, but the adsorption rate of active carbon is slack-off.When adsorption temp increases, the viscosity of sucrose is reduced, coloring matter
Diffusion velocity accelerate, be easy to adhere in activated carbon surface and its internal capillary, the adsorption rate of active carbon becomes faster.And when activity
When charcoal adsorption temp is 40~50 DEG C, it is big and obvious that medicinal grade cane sugar conductivity reduces amplitude.As adsorption temp is after of continuing rising
Height is become smaller with grade cane sugar conductivity reduction amplitude and is slowed down.And with the raising of activated carbon adsorption reaction temperature, the conversion speed of sucrose
Degree increases, therefore, to ensure the conductivity of medicinal grade cane sugar, to the control of production cost, the conversion for avoiding sucrose excessive, activity
The temperature of charcoal adsorption reaction is 50~70 DEG C.
4. the investigation of activated carbon adsorption time:
95% dehydrated alcohol for taking 43ml is added the ethanol solution of the deionized water configuration 55% of 40ml, configures 6 altogether
Part.Ethanol solution is separately heated to 55 DEG C, is separately added into 50g white granulated sugar and 0.5g active carbon, keep the temperature and stir 5min,
15min, 25min, 35min, 45min, 55min, filtering remove active carbon, and filtrate measures conductivity, the results are shown in Table four:
Table four: the investigation of different activities charcoal adsorption temp
Analysis: charted according to data in above table, as shown in figure 5, by Fig. 5 it is found that as activated carbon adsorption is reacted
The increase of time, medicinal grade cane sugar conductivity decrease.When active carbon is added within initial 25 minutes, medicinal grade cane sugar is electric
Conductance reduction amplitude is big and obvious, continues to extend with the activated carbon adsorption reaction time, the close saturation of activated carbon adsorptive capacity,
Medicinal grade cane sugar conductivity reduction amplitude, which becomes smaller, to slow down.To improve production efficiency, production cost is controlled, when activated carbon adsorption is reacted
Between be 25~35min.
5. recrystallizing concentration volume choice of parameters:
95% dehydrated alcohol for taking 43ml is added the ethanol solution of the deionized water configuration 55% of 40ml, configures 6 altogether
Part.Ethanol solution is separately heated to 55 DEG C, is separately added into 50g white granulated sugar and 0.5g active carbon, keeps the temperature and stir 35minn, mistake
Filter removes active carbon and obtains smoke filtrate.Smoke filtrate is -0.085MPa respectively at vacuum pressure, and temperature is 45 DEG C and is evaporated under reduced pressure to white sand
Sugar weight 110%, 120%, 130%, 140%, 150% (i.e. 1.1 times of White Sugar Quality, 1.2 times, 1.3 times, 1.4 times,
1.5 times), it is crystallized, is centrifuged, collect medicinal grade cane sugar, 45 DEG C of drying, weighing checks solution colour, the sulphur of medicinal grade cane sugar
Hydrochlorate, calcium salt, residue on ignition and heavy metal, the results are shown in Table four:
Table four: the investigation of different concentration volumes is recrystallized
Analysis: it is charted according to concentration volume in above table and the data of crystallization yield, as shown in fig. 6, by can in Fig. 6
Know, when sucrose recrystallization, volume is smaller after concentration, and crystallization of sucrose amount is more, but the precipitations such as sulfate, calcium salt become more, shadow therewith
Ring the quality of medicinal grade cane sugar.Crystallization darkens, and influences the color of medicinal grade cane sugar.Therefore, when recrystallization concentrate body
Product is 1.3~1.4 times of sucrose material weight, and the temperature of smoke filtrate concentration is 40~50 DEG C
In conclusion the ethanol solution concentration of activated carbon adsorption is 50~80%, sorption reaction time be 25~35min,
Active carbon additional amount is 0.6~0.8%, adsorption temp is 50~70 DEG C, and the crystallization concentration amount of recrystallization is sucrose material quality
1.3~1.4 times.
Embodiment 3:
Originally be embodiment it is optimal screening by the technical parameter of embodiment 2, medicine is prepared using the method for embodiment 1
Grade cane sugar, referring specifically to following three batches of pilot scales.
The neutral alcohol solution 750kg that dehydrated alcohol and deionized water configuration concentration with 95% are 60%, is added reaction
It is heated to 60 ± 2 DEG C in kettle, neutral hot ethanol solution is made；The sucrose material and 3kg of 500kg is added in neutral hot ethanol solution
Active carbon, carry out activated carbon adsorption reaction.60 ± 2 DEG C keep the temperature and stir 25min, cooling, obtain primary first-order equation liquid；To be once anti-
It answers liquid to filter and removes active carbon, obtain smoke filtrate；It is -0.085MPa that smoke filtrate is pressed in vacuum, and temperature depressurizes under the conditions of being 45 DEG C
It is concentrated by evaporation to the 700kg of sucrose material weight, obtains concentrate；It is recrystallized, is centrifuged at normal temperature, collect crystallization；It will knot
Crystalline substance crushed 80 meshes, weigh to obtain the medicinal grade cane sugar of 406.5kg after 45 DEG C of drying are dry.
It is detected, the yield for the medicinal grade cane sugar being refining to obtain is 81.3%, specific rotation 66.5, and conductivity is 18.5 μ
s/cm。
1. pilot scale first:
The neutral alcohol solution 600kg that dehydrated alcohol and deionized water configuration concentration with 95% are 75%, is added reaction
It is heated to 60 ± 2 DEG C in kettle, neutral hot ethanol solution is made；Neutral hot ethanol solution be added 300kg sucrose material and
The active carbon of 2.1kg carries out activated carbon adsorption reaction.55 ± 2 DEG C keep the temperature and stir 30min, cooling, obtain primary first-order equation liquid；It will
Primary first-order equation liquid, which filters, removes active carbon, obtains smoke filtrate；It is -0.085MPa that smoke filtrate is pressed in vacuum, and temperature is 45 DEG C of conditions
It is lower that the 390kg for being concentrated into sucrose material weight is evaporated under reduced pressure, obtain concentrate；It is recrystallized, is centrifuged at normal temperature, collect knot
It is brilliant；It will crystallize after 45 DEG C of drying are dry, and crushed 80 meshes, weigh to obtain the medicinal grade cane sugar of 253.5kg.
It is detected, the yield for the medicinal grade cane sugar being refining to obtain is 84.5%, specific rotation 66.7, and conductivity is 16.8 μ
s/cm。
2. pilot scale second batch:
The neutral alcohol solution 1000kg that dehydrated alcohol and deionized water configuration concentration with 95% are 80%, is added reaction
It is heated to 65 ± 2 DEG C in kettle, neutral hot ethanol solution is made；Neutral hot ethanol solution be added 500kg sucrose material and
The active carbon of 3.5kg carries out activated carbon adsorption reaction.67 ± 2 DEG C keep the temperature and stir 30min, cooling, obtain primary first-order equation liquid；It will
Primary first-order equation liquid, which filters, removes active carbon, obtains smoke filtrate；It is -0.085MPa that smoke filtrate is pressed in vacuum, and temperature is 45 DEG C of conditions
It is lower that the 650kg for being concentrated into sucrose material weight is evaporated under reduced pressure, obtain concentrate；It is recrystallized, is centrifuged at normal temperature, collect knot
It is brilliant；It will crystallize after 45 DEG C of drying are dry, and crushed 80 meshes, weigh to obtain the medicinal grade cane sugar of 425.5kg.
It is detected, the yield for the medicinal grade cane sugar being refining to obtain is 85.1%, specific rotation 66.1, and conductivity is 30.8 μ
s/cm。
3. pilot scale third batch:
The neutral alcohol solution 1000kg that dehydrated alcohol and deionized water configuration concentration with 95% are 80%, is added reaction
It is heated to 55 ± 2 DEG C in kettle, neutral hot ethanol solution is made；Neutral hot ethanol solution be added 500kg sucrose material and
The active carbon of 4.0kg carries out activated carbon adsorption reaction.60 ± 2 DEG C keep the temperature and stir 35min, cooling, obtain primary first-order equation liquid；It will
Primary first-order equation liquid, which filters, removes active carbon, obtains smoke filtrate；It is -0.085MPa that smoke filtrate is pressed in vacuum, and temperature is 45 DEG C of conditions
It is lower that the 650kg for being concentrated into sucrose material weight is evaporated under reduced pressure, obtain concentrate；It is recrystallized, is centrifuged at normal temperature, collect knot
It is brilliant；It will crystallize after 45 DEG C of drying are dry, and crushed 80 meshes, weigh to obtain the medicinal grade cane sugar of 410.5kg.
It is detected, the yield for the medicinal grade cane sugar being refining to obtain is 82.1%, specific rotation 66.4, and conductivity is 17.8 μ
s/cm。
The series of detailed descriptions listed above only for feasible embodiment of the invention specifically
Protection scope bright, that they are not intended to limit the invention, it is all without departing from equivalent implementations made by technical spirit of the present invention
Or change should all be included in the protection scope of the present invention.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (5)
1. a kind of process for refining of medicinal grade cane sugar, it is characterised in that: the following steps are included:
Step 1: 1.5 ~ 3 times of sucrose material weight of ethanol solution, the neutrality that ethanol solution is 40 ~ 90% are added in a kettle
Neutral alcohol solution is heated to 40 ~ 85 DEG C by ethanol solution, and neutral hot ethanol solution is made；
Step 2: 0.2 ~ 1.0% active carbon of sucrose material and sucrose material quality is added in neutral hot ethanol solution, carry out
Activated carbon adsorption reaction, 40 ~ 85 DEG C keep the temperature and stir 5 ~ 60min, cooling, obtain primary first-order equation liquid；
Active carbon is removed Step 3: primary first-order equation liquid is filtered, obtains smoke filtrate；
Step 4: smoke filtrate is concentrated into 1.2 ~ 1.5 times of sucrose material weight, concentrate is obtained；
Step 5: crystallization is collected in recrystallization, centrifugation；
Step 6: pulverizing and sieving after crystallizing and drying, medicinal grade cane sugar is obtained.
2. a kind of process for refining of medicinal grade cane sugar according to claim 1, it is characterised in that: in step 2, active carbon
Additional amount is the 0.6 ~ 0.8% of sucrose material.
3. a kind of process for refining of medicinal grade cane sugar according to claim 1, it is characterised in that: in step 1, ethyl alcohol is molten
Liquid concentration is 50 ~ 80%.
4. a kind of process for refining of medicinal grade cane sugar according to claim 1, it is characterised in that: in step 2, active carbon
The temperature of adsorption reaction is 50 ~ 70 DEG C, and the time is 25 ~ 35min.
5. a kind of process for refining of medicinal grade cane sugar according to claim 1, it is characterised in that: in step 4, recrystallization
When concentrate volume be 1.3 ~ 1.4 times of sucrose material weight, and the temperature of smoke filtrate concentration is 40 ~ 50 DEG C.
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Cited By (4)
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| WO2022029010A1 (en) * | 2020-08-07 | 2022-02-10 | Südzucker AG | Improved beet-sugar sucrose preparation |
| CN116143850A (en) * | 2022-12-22 | 2023-05-23 | 中粮崇左糖业有限公司 | Injection-grade sucrose, preparation method and application thereof |
| WO2024131789A1 (en) * | 2022-12-22 | 2024-06-27 | 中粮崇左糖业有限公司 | Injection-grade sucrose, preparation method, and use thereof |
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| CN111514180A (en) * | 2020-05-22 | 2020-08-11 | 贵州百灵企业集团制药股份有限公司 | Method for removing heavy metal ions in watermelon frost |
| WO2022029010A1 (en) * | 2020-08-07 | 2022-02-10 | Südzucker AG | Improved beet-sugar sucrose preparation |
| CN116143850A (en) * | 2022-12-22 | 2023-05-23 | 中粮崇左糖业有限公司 | Injection-grade sucrose, preparation method and application thereof |
| CN116143850B (en) * | 2022-12-22 | 2023-12-15 | 中粮崇左糖业有限公司 | Injection-grade sucrose, preparation method and application thereof |
| WO2024131789A1 (en) * | 2022-12-22 | 2024-06-27 | 中粮崇左糖业有限公司 | Injection-grade sucrose, preparation method, and use thereof |
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Address after: No.6, North tanbin Road, Fengjing Industrial Park, Guyi District, Xi'an City, Shaanxi Province Applicant after: Shaanxi Aoke pharmaceutical Accessories Co.,Ltd. Address before: No. 10, building 1, luowu lane, Lianhu District, Xi'an City, Shaanxi Province Applicant before: Shaanxi Aoke pharmaceutical Accessories Co.,Ltd. |
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Application publication date: 20191122 |