CN108570023A - A kind of ascorbic method of recycling - Google Patents
A kind of ascorbic method of recycling Download PDFInfo
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- CN108570023A CN108570023A CN201710140975.8A CN201710140975A CN108570023A CN 108570023 A CN108570023 A CN 108570023A CN 201710140975 A CN201710140975 A CN 201710140975A CN 108570023 A CN108570023 A CN 108570023A
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- thick
- recrystallization
- solution
- crystal
- mother liquors
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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)
- Saccharide Compounds (AREA)
Abstract
The invention discloses a kind of ascorbic methods of recycling, which is characterized in that it includes the following steps：Step 1 obtains VC recrystallization mother liquors from VC recrystallization processes with 10%~35% ratio, separately takes thick VC solution, VC recrystallization mother liquors and thick VC solution intake system are established Concentrated and crystallized in vacuum system；Step 2 is initially separated crystal when crystal is grown to 60 mesh in device to be crystallized, and VC is tied to mother liquor return system again, while continuous sucking VC recrystallization mother liquors, continuously sucking thick VC solution and carry out continuous condensing crystallizing and waste liquid is discharged；Step 3 starts that VC recrystallization mother liquors are discharged after continuously detaching 1,000 kilograms of thick VC crystal, and the thick VC crystal of gained can produce qualified finished product VC after re-crystallization after system stabilization.The present invention improves process recovery ratio, while reducing three waste discharge.
Description
Technical field
The present invention relates to a kind of recovery methods, more particularly to a kind of ascorbic method of recycling.
Background technology
At present workshop section, the mother after recrystallization separation finished product VC are recrystallized in the crude product VC of VC (vitamin C) production technology
Liquid is by continuing repeatedly to carry out the condensing crystallizing wherein remaining VC of extraction to mother liquor, in the technological operation of recycling this part VC
In due to scale it is smaller, the optimum process that VC solution condensing crystallizings are not achieved in recovery process is horizontal, as a result causes in this process
It is middle to be remained high by the VC ratios of Oxidative demage；And impurity concentration is all in product when being recycled each time in the VC solution of its concentration
What number rose, and impurity concentration can accelerate breakdown speeds of VC during condensing crystallizing after reaching certain level in VC solution,
(substantially condensing crystallizing three times) it is brilliant just can not successfully to obtain high-purity VC again after impurity concentration reaches a certain level wherein
Body；And this process portion causes the energy consumption level of process also can not effectively reduce due to scale is smaller, as a result causes whole
A VC production technologies level becomes a short slab in this part.Either recycle ratio or finally discharged quantity of three wastes all with reason
Think that there are larger gaps between state.
Invention content
Technical problem to be solved by the invention is to provide a kind of ascorbic methods of recycling, and VC crystalline mother solutions are returned
It is back to thick VC condensing crystallizings process, controls the impurity concentration progress condensing crystallizing of VC solution during thick VC condensing crystallizings, to
The withdrawal ratio for improving VC in original production process, reduces three waste discharge while improving process recovery ratio.
The present invention is to solve above-mentioned technical problem by following technical proposals：A kind of ascorbic method of recycling,
It is characterized in that comprising following steps：
Step 1 obtains VC recrystallization mother liquors from VC recrystallization processes with 10%~35% ratio, separately takes thick VC solution, will
VC recrystallization mother liquors establish Concentrated and crystallized in vacuum system with thick VC solution intake system；
Step 2 is initially separated crystal when crystal is grown to 60 mesh in device to be crystallized, and VC is tied to mother liquor return system again, together
Shi Lianxu sucking VC recrystallization mother liquors continuously suck thick VC solution progress continuous condensing crystallizing and waste liquid are discharged；
Step 3 starts that VC recrystallization mother liquors are discharged after continuously detaching 1,000 kilograms of thick VC crystal, after system stabilization
The thick VC crystal of gained can produce qualified finished product VC after re-crystallization.
Preferably, the step 2 continuously sucks VC recrystallization mother liquors, with 0.6m3/hr with the speed of 0.03m3/hr simultaneously
Speed continuously suck thick VC solution and carry out continuous condensing crystallizing and waste liquid is discharged.
Preferably, the speed of the step 3 discharge VC recrystallization mother liquors is 0.08m3/hr.
Preferably, VC contents are 12.0% in the VC recrystallization mother liquors of the step 3 discharge.
Preferably, the step 2 continuously sucks VC recrystallization mother liquors, with 0.6m3/hr with the speed of 0.06m3/hr simultaneously
Speed continuously suck thick VC solution and carry out continuous condensing crystallizing and waste liquid is discharged.
Preferably, the speed of the step 3 discharge VC recrystallization mother liquors is 0.04m3/hr.
Preferably, the speed of the step 3 discharge VC recrystallization mother liquors is 0.02m3/hr.
The positive effect of the present invention is that：Finished product VC crystalline mother solutions are back to thick VC condensing crystallizings work by the present invention
Sequence controls the impurity concentration progress condensing crystallizing of VC solution during thick VC condensing crystallizings, to improve VC in original production process
Withdrawal ratio, reduce three waste discharge while improving process recovery ratio.
Specific implementation mode
A kind of ascorbic method of recycling of the present invention includes the following steps：
Step 1 obtains VC recrystallization mother liquors from VC recrystallization processes with 10%~35% ratio, separately takes thick VC solution, will
VC recrystallization mother liquors establish Concentrated and crystallized in vacuum system with thick VC solution intake system；
Step 2 is initially separated crystal when crystal is grown to 60 mesh in device to be crystallized, and VC is tied to mother liquor return system again, together
Shi Lianxu sucking VC recrystallization mother liquors continuously suck thick VC solution progress continuous condensing crystallizing and waste liquid are discharged；
Step 3 starts that VC recrystallization mother liquors are discharged after continuously detaching 1,000 kilograms of thick VC crystal, after system stabilization
The thick VC crystal of gained can produce qualified finished product VC after re-crystallization.
Embodiment 1
Build similar condensing crystallizing equipment in pilot-scale and Patent No. CN101397286A Chinese patents, first with
10%~35% ratio obtains VC recrystallization mother liquor 3M3 from VC recrystallization processes, and wherein VC contents are 13.2%, separately take thick VC molten
Liquid 60M3, VC content is 18.3%, and VC recrystallization mother liquors 0.2M3 and thick VC solution 4M3 intake systems are established and are concentrated in vacuo
Crystallizing system；It is initially separated crystal when crystal is grown to 60 mesh in device to be crystallized, and VC is tied to mother liquor return system again, while with
The speed of 0.03m3/hr continuously sucks VC recrystallization mother liquors, continuously sucks thick VC solution progress continuously with the speed of 0.6m3/hr
Simultaneously waste liquid is discharged in condensing crystallizing；Start that VC recrystallization mother liquors are discharged after continuously detaching thick VC crystal 1000Kg, discharge VC is tied again
The speed of brilliant mother liquor is 0.08m3/hr, and VC contents are 12.0% in the VC recrystallization mother liquors of discharge, and gained is thick after system stabilization
VC crystal can produce qualified finished product VC after re-crystallization, and system yield is 92% at this time.The ratio of the waste liquid of discharge is
1%~15%.
Embodiment 2
The substance of embodiment 2 such as embodiment 1, VC recrystallization mother liquor suction velocities is adjusted to 0.06m3/hr, thick VC
The suction velocity of solution is constant, and the VC recrystallization mother liquor velocities of discharge are adjusted to 0.04m3/hr, and the thick VC of gained is in weight after system is stablized
Qualified finished product VC can be produced after crystallization, system yield is 96% at this time.
Embodiment 3
The substance of embodiment 3 such as embodiment 1, VC recrystallization mother liquors, the suction velocity of thick VC solution are all constant, by VC
The recrystallization mother liquor velocity of discharge is adjusted to 0.02m3/hr, and the thick VC of gained can equally be produced after re-crystallization after system is stablized
Qualified finished product VC, system yield is 98% at this time.
Thick VC is recrystallized the VC mother liquors after detaching finished product VC and returned in crude product VC stostes by the present invention, is extracted with former thick VC
Thick VC production processes, which synchronize, to be executed, and carrying out condensing crystallizing using the equipment in the Chinese patent of Patent No. CN101397286A obtains
To crude intermediate VC；Since the amount of crude product VC is sizable, in its extraction process concentration and crystallizer its produce energy
Power is all bigger, and destruction ratio when VC aqueous solutions are run in such devices suffered by VC is also up to current possibility
Minimum, the stability of each operating parameter is also fairly good, they can accurately control the end point values of each process, through to it
The analysis of operation matter state can also reach the matchless level of former equipment, can be from original for the extract yield to VC
94% come is improved to 98% or so, and mother liquor discharge ratio also original 15% is reduced to 8% or so, and the thick VC of gained
Content be also it is particularly stable, under normal operating conditions can continuous 120 hours or more its error within 2%；According to work
Skill runs the adjustment test of each parameter, at present under production level, mother liquor after thick VC aqueous solutions counterweight Crystallization Separation finished product VC
Optimum range there are one accommodating will appear the thick VC delustrings detection of gained substantially between 10% to 35% outside beyond the range
It is worth the case where higher or VC recycling ratios decline.
The foregoing describe the preferred embodiment for the present invention, and however, it is not to limit the invention, those skilled in the art couple
Embodiment disclosed herein can carry out improvement and the variation without departing from scope and spirit.
Claims (5)
1. a kind of ascorbic method of recycling, which is characterized in that it includes the following steps：Step 1, with 10%~35% ratio
Example obtains VC recrystallization mother liquors from VC recrystallization processes, thick VC solution is separately taken, by VC recrystallization mother liquors and thick VC solution intake system
Establish Concentrated and crystallized in vacuum system；Step 2 is initially separated crystal when crystal is grown to 60 mesh in device to be crystallized, and VC is tied mother again
Liquid return system, while continuously sucking VC recrystallization mother liquors, continuously sucking thick VC solution progress continuous condensing crystallizing and be discharged useless
Liquid；Step 3 starts that VC recrystallization mother liquors are discharged after continuously detaching 1,000 kilograms of thick VC crystal, and gained is thick after system stabilization
VC crystal can produce qualified finished product VC after re-crystallization.
2. a kind of ascorbic method of recycling according to claim 1, which is characterized in that the step 2 simultaneously with
The speed of 0.03m3/hr continuously sucks VC recrystallization mother liquors, continuously sucks thick VC solution progress continuously with the speed of 0.6m3/hr
Simultaneously waste liquid is discharged in condensing crystallizing.
3. a kind of ascorbic method of recycling according to claim 2, which is characterized in that the step 3 discharge VC weights
The speed of crystalline mother solution is 0.08m3/hr.
4. a kind of ascorbic method of recycling according to claim 1, which is characterized in that the VC of the step 3 discharge
VC contents are 12.0% in recrystallization mother liquor.
5. a kind of ascorbic method of recycling according to claim 1, which is characterized in that the step 3 discharge VC weights
The speed of crystalline mother solution is 0.02m3/hr.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710140975.8A CN108570023A (en) | 2017-03-10 | 2017-03-10 | A kind of ascorbic method of recycling |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710140975.8A CN108570023A (en) | 2017-03-10 | 2017-03-10 | A kind of ascorbic method of recycling |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108570023A true CN108570023A (en) | 2018-09-25 |
Family
ID=63578102
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710140975.8A Withdrawn CN108570023A (en) | 2017-03-10 | 2017-03-10 | A kind of ascorbic method of recycling |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108570023A (en) |
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2017
- 2017-03-10 CN CN201710140975.8A patent/CN108570023A/en not_active Withdrawn
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180925 |
|
| WW01 | Invention patent application withdrawn after publication |