CN103641804A - Method for recovering crystallization mother liquor of finished product vitamin C - Google Patents
Method for recovering crystallization mother liquor of finished product vitamin C Download PDFInfo
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- CN103641804A CN103641804A CN201310697596.0A CN201310697596A CN103641804A CN 103641804 A CN103641804 A CN 103641804A CN 201310697596 A CN201310697596 A CN 201310697596A CN 103641804 A CN103641804 A CN 103641804A
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- mother liquor
- recrystallization
- finished product
- thick
- solution
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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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for recovering crystallization mother liquor of finished product vitamin C (VC). The method comprises the following steps: 1, recrystallizing VC in proportion of 10 to 35% to obtain VC recrystallized mother liquor; additionally taking a coarse VC solution; and sucking the VC recrystallized mother liquor and the coarse VC solution into a system to establish a vacuum concentrating crystallizing system; 2, starting to separate crystals after the crystal grows to reach 60 meshes in a crystallizer; returning the VC recrystallized mother liquor to the system; continuously sucking VC recrystallized mother liquor and the coarse VC solution; continuously concentrating and crystallizing; and draining the waste liquor; and 3, starting to drain the VC recrystallized mother liquor after continuously separating out 1,000kg VC crystals; and then recrystallizing the obtained coarse VC crystals after the system is stabilized to obtain the qualified finished product VC. The method has the advantages that the VC extract ratio in the original production process is increased, the process recovery is increased, and the three-waste (waste gas, waste water and solid waste) emission is reduced.
Description
Technical field
The present invention relates to a kind of recovery method, particularly relate to a kind of method that reclaims finished product C-Crystals mother liquor.
Background technology
At present at VC(vitamins C) the crude product VC recrystallization workshop section of production technique, mother liquor after the separated finished product VC of its recrystallization is by continuing repeatedly mother liquor to be carried out to wherein remaining VC of condensing crystal extraction, in the technological operation of reclaiming this part VC because scale is smaller, recovery process does not reach the optimum process level of VC solution condensing crystal, and result causes the VC ratio of oxidized destruction in this operation high; And in its concentrated VC solution each time circulation time impurity concentration be all product and rise, and impurity concentration can be accelerated the breakdown speed of VC in condensing crystal process after reaching certain level in VC solution, after impurity concentration acquires a certain degree therein, (three condensing crystals substantially) just cannot successfully obtain high purity VC crystal again; And this part operation is because the energy consumption level that the less reason of scale causes operation also cannot effectively reduce, result causes whole VC production technique level to become a short slab at this part.That recovery ratio or finally discharged quantity of three wastes exist larger gap all and between perfect condition.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method that reclaims finished product C-Crystals mother liquor, it is back to thick VC condensing crystal operation by VC crystalline mother solution, control the impurity concentration of VC solution in thick VC condensing crystal process and carry out condensing crystal, thereby the withdrawal ratio of VC in raising original production process has reduced three waste discharge when improving process recovery ratio.
The present invention solves above-mentioned technical problem by following technical proposals: a kind of method that reclaims finished product C-Crystals mother liquor, it is characterized in that, and it comprises the following steps:
Step 1, the ratio with 10% ~ 35% obtains VC recrystallization mother liquor from VC recrystallization operation, separately gets thick VC solution, and VC recrystallization mother liquor and thick VC solution intake system are set up to Concentrated and crystallized in vacuum system;
Step 2, starts isolation of crystalline when crystal grows to 60 order in device to be crystallized, and VC is heavily tied to mother liquor retrieval system, sucks VC recrystallization mother liquor simultaneously continuously, sucks thick VC solution continuously and carry out continuous condensing crystallizing effluent discharge;
Step 3 starts to discharge VC recrystallization mother liquor at continuous separate after 1,000 kilograms, thick VC crystal, and after system stability, the thick VC crystal of gained can be produced qualified finished product VC after recrystallization.
Preferably, described step 2 is simultaneously with 0.03m
3the speed of/hr sucks VC recrystallization mother liquor continuously, with 0.6m
3the speed of/hr sucks continuously thick VC solution and carries out continuous condensing crystallizing effluent discharge.
Preferably, the speed of described step 3 discharge VC recrystallization mother liquor is 0.08m
3/ hr.
Preferably, in the VC recrystallization mother liquor that described step 3 is discharged, VC content is 12.0%.
Preferably, described step 2 is simultaneously with 0.06m
3the speed of/hr sucks VC recrystallization mother liquor continuously, with 0.6m
3the speed of/hr sucks continuously thick VC solution and carries out continuous condensing crystallizing effluent discharge.
Preferably, the speed of described step 3 discharge VC recrystallization mother liquor is 0.04m
3/ hr.
Preferably, the speed of described step 3 discharge VC recrystallization mother liquor is 0.02m
3/ hr.
Positive progressive effect of the present invention is: the present invention is back to thick VC condensing crystal operation by finished product VC crystalline mother solution, control the impurity concentration of VC solution in thick VC condensing crystal process and carry out condensing crystal, thereby the withdrawal ratio of VC in raising original production process has reduced three waste discharge when improving process recovery ratio.
Embodiment
The method that the present invention reclaims finished product C-Crystals mother liquor comprises the following steps:
Step 1, the ratio with 10% ~ 35% obtains VC recrystallization mother liquor from VC recrystallization operation, separately gets thick VC solution, and VC recrystallization mother liquor and thick VC solution intake system are set up to Concentrated and crystallized in vacuum system;
Step 2, starts isolation of crystalline when crystal grows to 60 order in device to be crystallized, and VC is heavily tied to mother liquor retrieval system, sucks VC recrystallization mother liquor simultaneously continuously, sucks thick VC solution continuously and carry out continuous condensing crystallizing effluent discharge;
Step 3 starts to discharge VC recrystallization mother liquor at continuous separate after 1,000 kilograms, thick VC crystal, and after system stability, the thick VC crystal of gained can be produced qualified finished product VC after recrystallization.
Embodiment 1
Building pilot scale and the patent No. is condensing crystal equipment close in CN101397286A Chinese patent, first with 10% ~ 35% ratio, from VC recrystallization operation, obtains VC recrystallization mother liquor 3M
3, wherein VC content is 13.2%, separately gets thick VC solution 60 M
3, its VC content is 18.3%, by VC recrystallization mother liquor 0.2 M
3with thick VC solution 4 M
3intake system is set up Concentrated and crystallized in vacuum system; When crystal grows to 60 order in device to be crystallized, start isolation of crystalline, and VC is heavily tied to mother liquor retrieval system, simultaneously with 0.03m
3the speed of/hr sucks VC recrystallization mother liquor continuously, with 0.6m
3the speed of/hr sucks continuously thick VC solution and carries out continuous condensing crystallizing effluent discharge; At continuous separate, after thick VC crystal 1000Kg, start to discharge VC recrystallization mother liquor, the speed of discharging VC recrystallization mother liquor is 0.08m
3/ hr, in the VC recrystallization mother liquor of discharge, VC content is 12.0%, and after system stability, the thick VC crystal of gained can be produced qualified finished product VC after recrystallization, and now system yield is 92%.The ratio of the waste liquid of discharging is 1% ~ 15%.
Embodiment 2
The substance of embodiment 2, as embodiment 1, is adjusted to 0.06m by VC recrystallization mother liquor suction velocity
3/ hr, the suction velocity of thick VC solution is constant, and the VC recrystallization mother liquor velocity of discharge is adjusted to 0.04 m
3/ hr, after system stability, the thick VC of gained can produce qualified finished product VC after recrystallization, and now system yield is 96%.
Embodiment 3
The substance of embodiment 3 is as embodiment 1, and the suction velocity of VC recrystallization mother liquor, thick VC solution is all constant, and the VC recrystallization mother liquor velocity of discharge is adjusted to 0.02 m
3/ hr, after system stability, the thick VC of gained can produce equally qualified finished product VC after recrystallization, and now system yield is 98%.
The present invention turns back to the VC mother liquor after the separated finished product VC of thick VC recrystallization in crude product VC stoste, extract thick VC production process with former thick VC and synchronize and carry out, utilize equipment in the Chinese patent that the patent No. is CN101397286A to carry out condensing crystal and obtain intermediate crude product VC, because the amount of crude product VC is sizable, in its extraction process, concentrated and its throughput of crystallizer is all larger, when the VC aqueous solution moves in these equipment, the suffered destruction ratio of VC has also reached possible Schwellenwert at present, the stability of each operating parameter is also goodish, they can accurately control the end point values of each operation, the matchless level of equipment before also can reaching the analysis of its operation matter state, the extract yield to VC just, can be increased to 98% left and right from original 94%, its mother liquor discharge ratio also original 15% is reduced to 8% left and right, and the content of the thick VC of gained is also to stablize especially, can be continuous under normal operating condition more than 120 hours its error in 2%, according to the adjustment test to each parameter of process operation, at present under production level, mother liquor after thick VC aqueous solution counterweight Crystallization Separation finished product VC accommodate an optimum range, roughly between 10% to 35%, there will be the situation that the thick VC delustring of gained detected value is higher or VC recovery ratio declines outward exceeding this scope.
More than described the preferred embodiment for the present invention, so it is not in order to limit the present invention, and those skilled in the art can not depart from improvement and the variation of category of the present invention and spirit to embodiment disclosed herein.
Claims (7)
1. a method that reclaims finished product C-Crystals mother liquor, is characterized in that, it comprises the following steps:
Step 1, the ratio with 10% ~ 35% obtains VC recrystallization mother liquor from VC recrystallization operation, separately gets thick VC solution, and VC recrystallization mother liquor and thick VC solution intake system are set up to Concentrated and crystallized in vacuum system;
Step 2, starts isolation of crystalline when crystal grows to 60 order in device to be crystallized, and VC is heavily tied to mother liquor retrieval system, sucks VC recrystallization mother liquor simultaneously continuously, sucks thick VC solution continuously and carry out continuous condensing crystallizing effluent discharge;
Step 3 starts to discharge VC recrystallization mother liquor at continuous separate after 1,000 kilograms, thick VC crystal, and after system stability, the thick VC crystal of gained can be produced qualified finished product VC after recrystallization.
2. the method for recovery finished product C-Crystals mother liquor as claimed in claim 1, is characterized in that, described step 2 is simultaneously with 0.03m
3the speed of/hr sucks VC recrystallization mother liquor continuously, with 0.6m
3the speed of/hr sucks continuously thick VC solution and carries out continuous condensing crystallizing effluent discharge.
3. the method for recovery finished product C-Crystals mother liquor as claimed in claim 2, is characterized in that, the speed that described step 3 is discharged VC recrystallization mother liquor is 0.08m
3/ hr.
4. the method for recovery finished product C-Crystals mother liquor as claimed in claim 1, is characterized in that, in the VC recrystallization mother liquor that described step 3 is discharged, VC content is 12.0%.
5. the method for recovery finished product C-Crystals mother liquor as claimed in claim 1, is characterized in that, described step 2 is simultaneously with 0.06m
3the speed of/hr sucks VC recrystallization mother liquor continuously, with 0.6m
3the speed of/hr sucks continuously thick VC solution and carries out continuous condensing crystallizing effluent discharge.
6. the method for recovery finished product C-Crystals mother liquor as claimed in claim 5, is characterized in that, the speed that described step 3 is discharged VC recrystallization mother liquor is 0.04m
3/ hr.
7. the method for recovery finished product C-Crystals mother liquor as claimed in claim 1, is characterized in that, the speed that described step 3 is discharged VC recrystallization mother liquor is 0.02m
3/ hr.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310697596.0A CN103641804A (en) | 2013-12-18 | 2013-12-18 | Method for recovering crystallization mother liquor of finished product vitamin C |
| CN201510348571.9A CN104945359A (en) | 2013-12-18 | 2013-12-18 | Method for recycling finished vitamin C crystallization mother liquor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310697596.0A CN103641804A (en) | 2013-12-18 | 2013-12-18 | Method for recovering crystallization mother liquor of finished product vitamin C |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510348571.9A Division CN104945359A (en) | 2013-12-18 | 2013-12-18 | Method for recycling finished vitamin C crystallization mother liquor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103641804A true CN103641804A (en) | 2014-03-19 |
Family
ID=50247129
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310697596.0A Pending CN103641804A (en) | 2013-12-18 | 2013-12-18 | Method for recovering crystallization mother liquor of finished product vitamin C |
| CN201510348571.9A Pending CN104945359A (en) | 2013-12-18 | 2013-12-18 | Method for recycling finished vitamin C crystallization mother liquor |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510348571.9A Pending CN104945359A (en) | 2013-12-18 | 2013-12-18 | Method for recycling finished vitamin C crystallization mother liquor |
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| CN (2) | CN103641804A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106587408A (en) * | 2016-12-09 | 2017-04-26 | 三达膜科技（厦门）有限公司 | Separation and concentration method of VB2 crystalline mother solution |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004007474A1 (en) * | 2002-07-12 | 2004-01-22 | Basf Aktiengesellschaft | Method for the separation of ascorbic acid from a polar solvent containing ascorbic acid and 2-keto-l-gulonic acid |
| DE10260085A1 (en) * | 2002-12-19 | 2004-07-01 | Basf Ag | Selective extraction of 2-keto-L-gulonic acid from polar solution, especially reaction mixture obtained in preparing ascorbic acid by lactonization, using mixture of tertiary amine and polar organic diluent |
| CN1690054A (en) * | 2004-04-23 | 2005-11-02 | 徐建涛 | Vitamine C refining process |
| CN101397286A (en) * | 2008-11-18 | 2009-04-01 | 江苏江山制药有限公司 | Method for continuous crystallisation of vitamin C |
| CN103254159A (en) * | 2013-01-29 | 2013-08-21 | 南京凯通粮食生化研究设计有限公司 | Vitamin C production process improvement method |
-
2013
- 2013-12-18 CN CN201310697596.0A patent/CN103641804A/en active Pending
- 2013-12-18 CN CN201510348571.9A patent/CN104945359A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004007474A1 (en) * | 2002-07-12 | 2004-01-22 | Basf Aktiengesellschaft | Method for the separation of ascorbic acid from a polar solvent containing ascorbic acid and 2-keto-l-gulonic acid |
| DE10260085A1 (en) * | 2002-12-19 | 2004-07-01 | Basf Ag | Selective extraction of 2-keto-L-gulonic acid from polar solution, especially reaction mixture obtained in preparing ascorbic acid by lactonization, using mixture of tertiary amine and polar organic diluent |
| CN1690054A (en) * | 2004-04-23 | 2005-11-02 | 徐建涛 | Vitamine C refining process |
| CN101397286A (en) * | 2008-11-18 | 2009-04-01 | 江苏江山制药有限公司 | Method for continuous crystallisation of vitamin C |
| CN103254159A (en) * | 2013-01-29 | 2013-08-21 | 南京凯通粮食生化研究设计有限公司 | Vitamin C production process improvement method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106587408A (en) * | 2016-12-09 | 2017-04-26 | 三达膜科技（厦门）有限公司 | Separation and concentration method of VB2 crystalline mother solution |
| CN106587408B (en) * | 2016-12-09 | 2019-11-05 | 三达膜科技（厦门）有限公司 | A kind of separation and concentration method of VB2 crystalline mother solution |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104945359A (en) | 2015-09-30 |
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Application publication date: 20140319 |