CN106831672A - A kind of decoloration treatment method of vitamine C sodium solution - Google Patents
A kind of decoloration treatment method of vitamine C sodium solution Download PDFInfo
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- CN106831672A CN106831672A CN201611270148.2A CN201611270148A CN106831672A CN 106831672 A CN106831672 A CN 106831672A CN 201611270148 A CN201611270148 A CN 201611270148A CN 106831672 A CN106831672 A CN 106831672A
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- resin
- treatment method
- sodium
- washed
- decoloration treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/56—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/62—Three oxygen atoms, e.g. ascorbic acid
Abstract
The invention provides a kind of decoloration treatment method of vitamine C sodium solution, belong to chemical field, the method of the present invention is to vitamine C sodium crude product obtained in Vc production alkali conversion procedures, directly it is configured to the aqueous solution, decolourized with the styrene D208 resin adsorptions containing pyridine groups, destainer is concentrated, crystallization, separate, dry, so as to the food-grade vitamine C sodium product of high-quality is obtained.The advantage of the invention is that cutting down the number of intermediate links, shorten process route, production cost is reduced, advantageously in industrial production.
Description
Technical field
The present invention relates to biological chemical field, specifically, being related to a kind of decoloration treatment method of vitamine C sodium solution.
Background technology
Vitamine C sodium is also referred to as L-AA sodium, and the effect of its preservation antioxidation substantially exceeds vitamin C, but valency
Lattice often only have ascorbic half, are widely used in the aspect of antistaling agent, medicine and the cosmetics of food etc..Changing
In work production, decolouring is very main technological process, so, decoloration process technology determines the quality of product.Current
In actual production, if it is desired to produce the good vitamine C sodium of mass, vitamin C must be first produced, but make dimension life
Plain C must will first produce the vitamin C of crude product, and the technological process of this method is long, and time-consuming, production cost
Height, is unfavorable for industrialized production, is further improved.
In vitamine C sodium, pigment is mainly fried sugar element and other organic compounds.Wherein fried sugar element essentially from
Many different organic compounds, also some are compound, sugarcane pigment and the pattern former times phenol of flavonoids.Other types color
The element product that usually sugar and coloring matter are reflected, also a kind of pigment, such as：Sugar has been made Jiao by heating degraded
Sugar.Decolourized easily to produce dust with activated carbon, and regenerating active carbon is very difficult, and its cost is also higher, can pollute week
The environment for enclosing, also wastes very much.
In vitamine C sodium production, shorten synthesis route, reduces cost just has great importance.Use resin
Desolventing technology is carried out to crude product vitamin C sodium solution, then by being recrystallized to give vitamine C sodium, this processing method is that have
Sizable meaning.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of decoloration treatment method of vitamine C sodium solution.
The purpose of the present invention is directly to produce alkali conversion procedure with Vc vitamine C sodium crude product is obtained, and produces the dimension of food-grade
Raw element C sodium, shortens process route, saves production cost, more conducively industrialized production.
Present invention firstly provides a kind of decoloration treatment method of solution of organic compound, comprise the following steps：
(1) macroreticular resin is pre-processed；
(2) the solution of organic compound mixing after pretreated macroreticular resin and filtering and impurity removing, constant temperature oscillation；
(3) resin is filtered out for regenerating；Filtrate is by concentrating, crystallizing, separate, dry.
Further, a kind of decoloration treatment method of vitamine C sodium solution that the present invention is provided, comprises the following steps：
(1) macroreticular resin is pre-processed；
(2) the crude vitamin C sodium solution mixing after pretreated macroreticular resin and filtering and impurity removing, constant temperature oscillation；
(3) resin is filtered out for regenerating；Filtrate can obtain finished product vitamin after concentrating, crystallizing, separate, dry
C sodium.
In the above method, step (1) macroreticular resin preprocess method includes step：
1) soaked in absolute ethyl alcohol is used, is washed；
2) soaked with sodium hydroxide solution, washing；
3) salt acid soak is used, is washed；
4) resin is collected by filtration and dries.
Step 1) the soaked in absolute ethyl alcohol time is 15-25h, is then washed with water to pH value neutral.
Step 2) concentration of sodium hydroxide solution be 0.1-0.4mol/L, soak 4-5h；It is washed with water to pH value neutral.
Step 3) concentration of hydrochloric acid be 0.1-0.4mol/L, soak 4-5h；It is washed with water to pH value neutral.
The present invention provide vitamine C sodium solution decoloration treatment method in, step (2) pretreated macroreticular resin and
The mass volume ratio of the crude vitamin C sodium solution mixing after filtering and impurity removing is 1:50-100g/ml mixes.
Preferably, the matter of the crude vitamin C sodium solution mixing after step (2) pretreated macroreticular resin and filtering and impurity removing
Amount volume ratio is 1:70-80g/ml mixes.
The condition of step (2) constant temperature oscillation is 15-50 in the decoloration treatment method of the vitamine C sodium solution that the present invention is provided
DEG C, vibrate 1-7h.
Preferably, the condition of step (2) constant temperature oscillation is 25-35 DEG C, vibrates 4-5h, 80-150 times/min of frequency of oscillation.
It is preferred that 100 times/min of frequency of oscillation.
Step (3) filter out resin for regenerate processing method be：Resin is washed with deionized 2-5 times, with 2-4 times
The 0.01-0.05mol/L dilute sulfuric acids of resin volume are processed resin, are washed with deionized to neutrality, with 2-4 times of resin
The 0.05-0.1mol/L sodium hydroxide solutions of volume and isometric mixture of 0.1-0.5mol/L sodium chloride solutions are in 50-70
Washed 2-5 times at a temperature of DEG C, be then washed with deionized to neutrality；Resin after washing filter and then dried, you can
Recycling.
Compared with prior art, the inventive method saves the middle process of vitamine C sodium synthesis, shortens technique road
Line, greatly improves production efficiency and utilization rate of equipment and installations.The present invention produces vitamine C sodium finished appearance brilliant white, purity
Height, the crystalline content of needle-like is more than 98%.Macroreticular resin is renewable in the present invention reuses greatly reduced cost.D208
The percent of decolourization of resin reaches more than 80%, 101 ° -103 ° of the finished product optical activity after treatment.
Specific embodiment
Following examples further illustrate present disclosure, but should not be construed as limiting the invention.Without departing substantially from
In the case of spirit of the invention and essence, the modification or replacement made to the inventive method, step or condition belong to the present invention
Scope.
If not specializing, the conventional meanses that technological means used is well known to those skilled in the art in embodiment.
Resin used by the present invention is the styrene D208 resins containing pyridine groups.
The decoloration treatment method (1) of the vitamine C sodium solution of embodiment 1
The D208 resins for taking 2.0g are loaded in exchange column, with 15ml soaked in absolute ethyl alcohol 15h.Then deionized water is used
15ml points of 2 washing is neutral to pH, then soaks 4h with 2 times of resin volume NaOH (0.1mol/L) solution.Then spend from
Sub- water 100ml points of 4 washing soaks 4h to neutrality with 2 times of resin volume HCl (0.1mol/L) solution, uses 100ml deionized waters
Divide 4 washings neutral to pH, be collected by filtration standby for desolventing technology after resin is dried.Measure the thick dimension through filtering and impurity removing of 70ml
Raw element C sodium solutions are weighed in dried resin 1.0g additions conical flask again in the conical flask of 250ml, then, in 25 DEG C of water
5h, the frequency (100 times/min) of vibration are vibrated under bath temperature.After vibration terminates, regeneration of the resin for resin is filtered out with filter paper
It is standby, finished product vitamine C sodium is then recrystallized to give to filtrate.The recycling of resin deionized water 100ml washing resins 2
It is secondary, resin is processed with 2 times of resin volume dilute sulfuric acids (0.01mol/L), with deionized water 100ml points of 2 washing into
Property, with 2 times of resin volume sodium hydroxide solutions (0.1mol/L) and mixture (both bodies of sodium chloride solution (0.5mol/L)
Product is than being 1:1) 2 times are washed at 50 DEG C, then deionized water 100ml points is washed to neutrality 2 times.Resin after washing is taken out
Filter, dry, you can recycling.The finished product vitamine C sodium detection data for obtaining reaches the requirement of food-grade vitamine C sodium, makes
Resin after can also be reused by treatment and not influence product quality.Purity reaches 99%, acicular crystal content
98.2%, 102 ° of finished product optical activity.
The decoloration treatment method (2) of the vitamine C sodium solution of embodiment 2
The D208 resins for taking 2.0g are loaded in exchange column, with 15ml soaked in absolute ethyl alcohol 16h.Then deionized water is used
Points of 2 times washings of 10ml are 7 to pH, then soak 5h with 2.5 times of resin volume NaOH (0.15mol/L) solution.Then spend
Ionized water 75ml points of 2 washing pH are 7, and 5h is soaked with 2.5 times of resin volume HCl (0.15mol/L) solution, use deionized water
75ml points of 2 washing pH are 7, are collected by filtration standby for desolventing technology after resin is dried.Measure 75ml through the thick of filtering and impurity removing
Vitamine C sodium solution in the conical flask of 250ml, then weigh 1.0g dry after resin be added thereto, in 30 DEG C of bath temperature
Lower vibration 5h, the frequency (100 times/min) of vibration after vibration terminates, resin is filtered out with filter paper, then to filtrate recrystallization just
Finished product vitamine C sodium can be obtained.The recycling of resin deionized water 75ml washing resins 3 times, with 3 times of resin volumes
Dilute sulfuric acid (0.015mol/L) is processed resin, is 7 with points of 3 times washing pH of deionized water 75ml, with 3 times of resin volumes
The mixture of sodium hydroxide solution (0.1mol/L) and sodium chloride solution (0.5mol/L) 55 DEG C wash 3 times, then spend from
It is 7 that sub- water 75ml washes pH points for 3 times, and the resin after washing is carried out into suction filtration, drying, you can recycling.The finished product dimension life for obtaining
Plain C sodium detection data reaches the requirement of food-grade vitamine C sodium, and the resin after use can also reuse not shadow by treatment
Ring product quality.Purity reaches 99.5%, acicular crystal content 98.3%, 103 ° of finished product optical activity.
Embodiment 3-dimensional gives birth to the decoloration treatment method (3) of element C sodium solutions
Crude product vitamin C sodium solution in embodiment 1 is changed to 80ml, duration of oscillation is changed to 4h, remaining is with implementation case
Example 1, the finished product vitamine C sodium detection data for obtaining reaches the requirement of food-grade vitamine C sodium, and the resin after use is by treatment
Can also reuse without influence product quality, the vitamine C sodium purity for obtaining be 99%, acicular crystal content 98% with
On, 101 ° of finished product optical activity.
The decoloration treatment method (4) of the vitamine C sodium solution of embodiment 4
The temperature that case study on implementation 1 vibrates is changed to 35 DEG C, duration of oscillation is changed to 4.5h, remaining is obtained with case study on implementation 1
Finished product vitamine C sodium detection data reach the requirement of food-grade vitamine C sodium, the resin after use can also be again by treatment
Secondary use is without influence product quality, the vitamine C sodium purity for obtaining and acicular crystal content, finished product optical activity and embodiment 1
It is similar.
The decoloration treatment method (5) of the vitamine C sodium solution of embodiment 5
The volume of the sodium hydroxide solution that case study on implementation 1 is used is changed to 4 times, and the concentration of sodium hydroxide solution is changed to
0.2mol/L,, with case study on implementation 1, the finished product vitamine C sodium detection data for obtaining reaches wanting for food-grade vitamine C sodium for remaining
Ask, the resin after use can also be reused without influence product quality, the vitamine C sodium purity and pin for obtaining by treatment
Shape crystalline content, finished product optical activity are similar with the result of embodiment 1.
It can be seen that the inventive method can be very good for Vc to produce alkali conversion procedure system in case study on implementation more than
Obtain vitamine C sodium crude product and finished product vitamine C sodium is obtained by the desolventing technology of D208 resins, the resin used in decolorization is passed through
Crossing simple treatment can repeat using multiple, while greatly shortening the route of technique and the cost of production.This hair
The bright fried sugar element for applying also for organic matter generation and other organic compound pigments (are the products of sugar and the reaction of coloring matter premise
Thing) etc. desolventing technology.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. a kind of decoloration treatment method of solution of organic compound, it is characterised in that comprise the following steps：
(1) macroreticular resin is pre-processed；
(2) the solution of organic compound mixing after pretreated macroreticular resin and filtering and impurity removing, constant temperature oscillation；
(3) resin is filtered out for regenerating；Filtrate is by concentrating, crystallizing, separate, dry.
2. decoloration treatment method as claimed in claim 1, it is characterised in that described solution of organic compound is vitamin C
Sodium solution.
3. decoloration treatment method as claimed in claim 1, it is characterised in that step (1) macroreticular resin preprocess method includes
Step：
1) soaked in absolute ethyl alcohol is used, is washed；
2) soaked with sodium hydroxide solution, washing；
3) salt acid soak is used, is washed；
4) resin is collected by filtration and dries.
4. decoloration treatment method as claimed in claim 3, it is characterised in that step 1) the soaked in absolute ethyl alcohol time is 15-
25h, is then washed with water to pH value neutral.
5. decoloration treatment method as claimed in claim 3, it is characterised in that step 2) concentration of sodium hydroxide solution is 0.1-
0.4mol/L, soaks 4-5h；It is washed with water to pH value neutral.
6. decoloration treatment method as claimed in claim 3, it is characterised in that step 3) concentration of hydrochloric acid is 0.1-0.4mol/L,
Immersion 4-5h；It is washed with water to pH value neutral.
7. the decoloration treatment method as described in claim 2-6 is any, it is characterised in that the pretreated macropore tree of step (2)
The mass volume ratio of the crude vitamin C sodium solution mixing after fat and filtering and impurity removing is 1:50-100 (g/ml) mixes.
8. the decoloration treatment method as described in claim 2-6 is any, it is characterised in that the condition of step (2) constant temperature oscillation is
15-50 DEG C, vibrate 1-7h.
9. decoloration treatment method as claimed in claim 8, it is characterised in that the condition of step (2) constant temperature oscillation is 25-35
DEG C, vibrate 4-5h, 80-150 times/min of frequency of oscillation.
10. the decoloration treatment method as described in claim 1-6 is any, it is characterised in that step (3) filters out resin for again
Raw processing method is：Resin is washed with deionized 2-5 times, with the 2-4 times of 0.01-0.05mol/L dilute sulfuric acid of resin volume
Resin is processed, is washed with deionized to neutrality, the 0.05-0.1mol/L NaOH with 2-4 times of resin volume is molten
Isometric mixture of liquid and 0.1-0.5mol/L sodium chloride solutions is washed 2-5 times at a temperature of 50-70 DEG C, then uses deionization
Water washing is to pH 6-8；Resin after washing filter and then dried, you can recycling.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611270148.2A CN106831672A (en) | 2016-12-30 | 2016-12-30 | A kind of decoloration treatment method of vitamine C sodium solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611270148.2A CN106831672A (en) | 2016-12-30 | 2016-12-30 | A kind of decoloration treatment method of vitamine C sodium solution |
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| CN106831672A true CN106831672A (en) | 2017-06-13 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1116202A (en) * | 1995-04-19 | 1996-02-07 | 江西赣江制药有限责任公司 | Purifying method for L-sodium ascorbate |
| CN101550118A (en) * | 2009-05-22 | 2009-10-07 | 徐建涛 | Synthetic process for vitamin C sodium salts |
| CN103102335A (en) * | 2012-11-15 | 2013-05-15 | 江苏江山制药有限公司 | Method for producing crude sodium L-ascorbate by recovering crude vitamin C mother liquor |
| CN104557822A (en) * | 2015-01-19 | 2015-04-29 | 精晶药业股份有限公司 | Refinement method of vitamin C sodium salt |
-
2016
- 2016-12-30 CN CN201611270148.2A patent/CN106831672A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1116202A (en) * | 1995-04-19 | 1996-02-07 | 江西赣江制药有限责任公司 | Purifying method for L-sodium ascorbate |
| CN101550118A (en) * | 2009-05-22 | 2009-10-07 | 徐建涛 | Synthetic process for vitamin C sodium salts |
| CN103102335A (en) * | 2012-11-15 | 2013-05-15 | 江苏江山制药有限公司 | Method for producing crude sodium L-ascorbate by recovering crude vitamin C mother liquor |
| CN104557822A (en) * | 2015-01-19 | 2015-04-29 | 精晶药业股份有限公司 | Refinement method of vitamin C sodium salt |
Non-Patent Citations (2)
| Title |
|---|
| 李青等: "大孔树脂对维生素C 钠的脱色研究", 《河北工业科技》 * |
| 高生彬等: "大孔吸附树脂对维生素C脱色研究", 《河北化工》 * |
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Application publication date: 20170613 |