Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide one to utilize heavy phase lactic acid to produce continuously Lactated method, most of lactic acid extraction in heavy phase lactic acid can be obtained to the lactic acid salt aqueous solution in organic phase and after alkaline solution is stripped, make to utilize heavy phase lactic acid can produce fine purification of lactic acid salt or lactic acid, and operational path is simple, production cost is low.
Technical scheme of the present invention is achieved in that utilizes heavy phase lactic acid to produce continuously Lactated method, comprises the steps:
(a) dilution: the massfraction that heavy phase lactic acid is diluted to lactic acid is 10-60%;
(b) charcoal post decolouring: loaded particles charcoal in charcoal post, obtains heavy phase lactic acid to be extracted after the decolouring of charcoal post;
(c) extraction: organic extraction is made up of extraction agent, solvent and phase modifier, extraction agent is the mixture of amides or amides, solvent is whiteruss, phase modifier is the mixture of alcohol compound or alcohol compound, extraction agent, solvent and phase modifier three's mass ratio (5.5-6.5): (2.5-3.5): (0.5-1); Organic extraction phase is (1.1-1.5) with the mass ratio of heavy phase lactic acid to be extracted: 1, and extracting operation temperature is 20-70 DEG C; Lactic acid is transferred to selectively in organic extraction mutually and formed load organic phases, make the impurity in heavy phase lactic acid obtain effective separation with lactic acid; Water is after reverse osmosis membrane processing, and dialyzate is used for diluting initial feed heavy phase lactic acid; Concentrated solution decomposes in IC bio-reactor produces biogas, for the thermal source of feed drying;
(d) strip: strippant is the suspension liquid of alkaline solution or alkali, and reextraction temperature is 20-30 DEG C; Load organic phases obtains the lactic acid salt aqueous solution after alkaline solution is stripped;
(e) essence filter: utilize the filter of particle charcoal post essence decolour and remove impurity;
(f) concentrated: after adopting multiple-effect evaporator concentrated, to obtain lactate solution.
The above-mentioned heavy phase lactic acid that utilizes is produced Lactated method continuously, and described alkali is the alkali that basic metal or alkaline-earth metal form.Basic metal is lithium, sodium or potassium, and the alkali of formation is lithium hydroxide, sodium hydroxide and potassium hydroxide; Alkaline-earth metal is magnesium or calcium, and the alkali of formation is magnesium hydroxide and calcium hydroxide, and transition metal is iron, zinc, copper or aluminium, and the alkali of formation is ferrous hydroxide, zinc hydroxide, copper hydroxide and aluminium hydroxide.
The above-mentioned heavy phase lactic acid that utilizes is produced Lactated method continuously, and described alkaline solution is sodium hydroxide solution, and in sodium hydroxide solution, the massfraction of sodium hydroxide is 25-31%.
The above-mentioned heavy phase lactic acid that utilizes is produced Lactated method continuously, and described alkaline solution is potassium hydroxide solution, and in potassium hydroxide solution, the massfraction of potassium hydroxide is 30-45%.
The above-mentioned heavy phase lactic acid that utilizes is produced Lactated method continuously, and described alkaline solution is calcium hydroxide suspension liquid, and in calcium hydroxide suspension liquid, the massfraction of calcium hydroxide is 8-20%.
The above-mentioned heavy phase lactic acid that utilizes is produced Lactated method continuously, and in load organic phases, the amount of substance concentration of lactic acid is 0.5-0.9mol/L.
The above-mentioned heavy phase lactic acid that utilizes is produced continuously Lactated method, and in strippant, in amount of substance hydroxy and load organic phases, the ratio of the amount of substance of lactic acid is (0.8-0.95): 1.
The above-mentioned heavy phase lactic acid that utilizes is produced Lactated method continuously, and the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 20%-30%; The middle extraction agent of step (c), solvent and phase modifier three's mass ratio 6: 3: 0.8; Organic extraction phase is 1.15: 1 with the mass ratio of heavy phase lactic acid to be extracted, and temperature is 30-45 DEG C.
The above-mentioned heavy phase lactic acid that utilizes is produced Lactated method continuously, and in step (c), the time of balancing each other is 25-50min.
The above-mentioned heavy phase lactic acid that utilizes is produced Lactated method continuously, and amides has as shown in the formula the structure shown in (I):
Wherein R1 is hydrogen, chain alkylene or alicyclic hydrocarbon radical, and R2 is hydrogen, chain alkylene or alicyclic hydrocarbon radical, and R3 is hydrogen, chain alkylene or alicyclic hydrocarbon radical.
The above-mentioned heavy phase lactic acid that utilizes is produced Lactated method continuously, and R1, R2 and R3 are alkyl.
The above-mentioned heavy phase lactic acid that utilizes is produced Lactated method continuously, and alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, chain alkylene or alicyclic hydrocarbon radical, and R5 is hydrogen, chain alkylene or alicyclic hydrocarbon radical, and R6 is chain alkylene or alicyclic hydrocarbon radical.
The invention has the beneficial effects as follows: the present invention looks for another way, adopting heavy phase lactic acid is raw material production lactic acid and lactic acid salt, add organic extraction phase, lactic acid is transferred to organic phase selectively and form load organic phases and obtain the lactic acid salt aqueous solution after the suspension liquid of alkaline solution or alkali is stripped, make impurity and lactic acid obtain effective separation.Adopting heavy phase lactic acid is raw material, has solved the restraining factors of purified grade lactic acid, and resource is rationally utilized.
Embodiment
embodiment 1
In the present embodiment, utilizing heavy phase lactic acid to produce continuously Lactated method comprises the steps:
(a) dilution: the massfraction that heavy phase lactic acid is diluted to lactic acid is 20%;
(b) charcoal post decolouring: loaded particles charcoal in charcoal post, obtains heavy phase lactic acid to be extracted after the decolouring of charcoal post;
(c) extraction: organic extraction is made up of extraction agent, solvent and phase modifier, and extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.Amides has as shown in the formula the structure shown in (I):
Wherein R1 is CH
3(CH
2)
3-, R2 is hydrogen, R3 is CH
3(CH
2)
3-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH
3cH
2-.
Extraction agent, solvent and phase modifier three's mass ratio 5.5: 2.5: 0.5; Organic extraction phase is 1.1: 1 with the mass ratio of heavy phase lactic acid to be extracted, and extracting operation temperature is 30 DEG C, organic extraction phase is fully mixed with heavy phase lactic acid to be extracted, and stratification, the time of balancing each other is 30min; In water, lactic acid massfraction is 0.5%.Lactic acid is transferred to selectively in organic extraction mutually and formed load organic phases, make the impurity in heavy phase lactic acid obtain effective separation with lactic acid; Water is after reverse osmosis membrane processing, and dialyzate is used for diluting initial feed heavy phase lactic acid; Concentrated solution decomposes in IC bio-reactor produces biogas, for the thermal source of feed drying.
(d) strip: strippant [sodium hydroxide solution] and load organic phases are mixed and reacted in pipeline reactor, after mixing, injecting reactor strips, concrete technology parameter is as shown in table 1, and [C represents the concentration of lactic acid in load organic phases, W represents the massfraction of sodium hydroxide in sodium hydroxide solution, N
1represent amount of substance hydroxy in sodium hydroxide solution, N
2represent the amount of substance of lactic acid in load organic phases]:
Load organic phases obtains sodium lactate aqueous solution after sodium hydroxide solution is stripped, stripping rate in table 1 represent the alkali reaction in lactic acid and the strippant in load organic phases and enter into strippant ratio [as: table 1 experiment numbers 1 stripping rate is 80%, represents to have in load organic phases 80% lactic acid to react generation Sodium.alpha.-hydroxypropionate with sodium hydroxide];
(e) essence filter: utilize the filter of particle charcoal post essence decolour and remove impurity;
(f) concentrated: after adopting vaporizer concentrated, to obtain lactate solution.
embodiment 2
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 30%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 6.5: 3.5: 1.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is (CH
2)
5cH-, R2 is hydrogen, R3 is CH
3(CH
2)
7-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH
3(CH
2)
5-.
Be 1.5: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase,, extracting operation temperature is 33 DEG C, stratification, the time of balancing each other is 36min; In water, lactic acid massfraction is 0.4%.
In step (d): strippant [sodium hydroxide solution] and load organic phases are mixed in pipeline reactor, after mixing, injecting reactor strips, concrete technology parameter is as shown in table 2, and [C represents the concentration of lactic acid in load organic phases, W represents the massfraction of sodium hydroxide in sodium hydroxide solution, N1 represents amount of substance hydroxy in sodium hydroxide solution, and N2 represents the amount of substance of lactic acid in load organic phases]:
embodiment 3
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 25%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 6: 3: 0.8.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is CH
3(CH
2)
9-, R2 is hydrogen, R3 is CH
3(CH
2)
6-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH
3cH
2-.
Be 1.3: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 33 DEG C, stratification, and the time of balancing each other is 50min; In water, lactic acid massfraction is 0.3%.
In step (d): strippant [sodium hydroxide solution] and load organic phases are mixed in pipeline reactor, after mixing, injecting reactor strips, concrete technology parameter is as shown in table 3, and [C represents the concentration of lactic acid in load organic phases, W represents the massfraction of sodium hydroxide in sodium hydroxide solution, N
1represent amount of substance hydroxy in sodium hydroxide solution, N
2represent the amount of substance of lactic acid in load organic phases]:
embodiment 4
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 28%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 5.7: 3.2: 0.7.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is (CH
3)
2cHCH
2cH (CH
2cH
3) CH
2-, R2 is CH
3(CH
2)
2-, R3 is (CH
3)
2cHCH (CH
3) CH
2-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH
3cH
2cH (CH
3) CH
2-.
Be 1.2: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 45 DEG C, stratification, and the time of balancing each other is 45min; In water, lactic acid massfraction is 0.5%.
In step (d): strippant [sodium hydroxide solution] and load organic phases are mixed in pipeline reactor, after mixing, injecting reactor strips, concrete technology parameter is as shown in table 4, and [C represents the concentration of lactic acid in load organic phases, W represents the massfraction of sodium hydroxide in sodium hydroxide solution, N
1represent amount of substance hydroxy in sodium hydroxide solution, N
2represent the amount of substance of lactic acid in load organic phases]:
embodiment 5
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 21%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 6.2: 2.8: 0.6.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is CH
3cH (CH
3) CH
2-, R2 is CH
3-, R3 is CH
3(CH
2)
2cH (CH
3) (CH
2)
2-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH
3(CH
2)
2-.
Be 1.4: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 40 DEG C, stratification, and the time of balancing each other is 30min; In water, lactic acid massfraction is 0.3%.
In step (d): strippant [potassium hydroxide solution] and load organic phases are mixed in pipeline reactor, after mixing, injecting reactor strips, concrete technology parameter is as shown in table 5, and [C represents the concentration of lactic acid in load organic phases, W represents the massfraction of potassium hydroxide in potassium hydroxide solution, N
1represent amount of substance hydroxy in potassium hydroxide solution, N
2represent the amount of substance of lactic acid in load organic phases]:
embodiment 6
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 28%; In step (c); Extraction agent, solvent and phase modifier three's mass ratio 6: 3: 0.8.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is CH
3(CH
2)
9-, R2 is CH
3cH
2-, R3 is CH
3(CH
2)
2cH (CH
3) (CH
2)
2-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is CH
3-, R5 is hydrogen, R6 is CH
3(CH
2)
2-.
Be 1.3: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 36 DEG C, stratification, and the time of balancing each other is 40min; In water, lactic acid massfraction is 0.5%.
In step (d): strippant [potassium hydroxide solution] and load organic phases are mixed in pipeline reactor, after mixing, injecting reactor strips, concrete technology parameter is as shown in table 6, and [C represents the concentration of lactic acid in load organic phases, W represents the massfraction of potassium hydroxide in potassium hydroxide solution, N
1represent amount of substance hydroxy in potassium hydroxide solution, N
2represent the amount of substance of lactic acid in load organic phases]:
embodiment 7
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 26%; In step (c); Extraction agent, solvent and phase modifier three's mass ratio 6.5: 3.5: 1.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is CH
3cH (CH
3) CH
2-, R2 is CH
3cH
2-, R3 is CH
3(CH
2)
1-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH
3(CH
2)
5-.
Be 1.25: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 31 DEG C, stratification, and the time of balancing each other is 35min; In water, lactic acid massfraction is 0.7%.
In step (d): strippant [potassium hydroxide solution] and load organic phases are mixed in pipeline reactor, after mixing, injecting reactor strips, concrete technology parameter is as shown in table 7, and [C represents the concentration of lactic acid in load organic phases, W represents the massfraction of potassium hydroxide in potassium hydroxide solution, N
1represent amount of substance hydroxy in potassium hydroxide solution, N
2represent the amount of substance of lactic acid in load organic phases]:
embodiment 8
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 24%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 6.5: 2.5: 1.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is (CH
3)
2cHCH
2cH (CH
2cH
3) CH
2-, R2 is hydrogen, R3 is (CH
3)
2cHCH (CH
3) CH
2-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is CH
3-, R5 is hydrogen, R6 is CH
3cH
2-.
Be 1.15: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 33 DEG C, stratification, and the time of balancing each other is 30min; In water, lactic acid massfraction is 0.2%.
In step (d): strippant [potassium hydroxide solution] and load organic phases are mixed in pipeline reactor, after mixing, injecting reactor strips, concrete technology parameter is as shown in table 8, and [C represents the concentration of lactic acid in load organic phases, W represents the massfraction of potassium hydroxide in potassium hydroxide solution, N
1represent amount of substance hydroxy in potassium hydroxide solution, N
2represent the amount of substance of lactic acid in load organic phases]:
embodiment 9
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 22%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 5.5: 3: 0.5.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is (CH
2)
5cH-, R2 is CH
3-, R3 is (CH
2)
5cH-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH
3cH
2cH (CH
3) CH
2-.
Be 1.23: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 38 DEG C, stratification, and the time of balancing each other is 40min; In water, lactic acid massfraction is 0.7%.
In step (d): strippant [calcium hydroxide suspension liquid] and load organic phases are mixed in pipeline reactor, after mixing, injecting reactor strips, concrete technology parameter is as shown in table 9, and [C represents the concentration of lactic acid in load organic phases, W represents the massfraction of calcium hydroxide in calcium hydroxide suspension liquid, N
1represent amount of substance hydroxy in calcium hydroxide suspension liquid, N
2represent the amount of substance of lactic acid in load organic phases]:
embodiment 10
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 27%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 6: 3: 0.8.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is CH
1(CH
2)
3-, R2 is hydrogen, R3 is (CH
2)
5cHCH
2-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH
3cH
2cH (CH
3) CH
2-.
Be 1.36: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 37 DEG C, stratification, and the time of balancing each other is 25min; In water, lactic acid massfraction is 0.5%.
In step (d): strippant [calcium hydroxide suspension liquid] and load organic phases are mixed in pipeline reactor, after mixing, injecting reactor strips, concrete technology parameter is as shown in table 10, and [C represents the concentration of lactic acid in load organic phases, W represents the massfraction of calcium hydroxide in calcium hydroxide suspension liquid, N
1represent amount of substance hydroxy in calcium hydroxide suspension liquid, N
2represent the amount of substance of lactic acid in load organic phases]:
embodiment 11
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 26.5%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 6: 3: 0.8.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is CH
3(CH
2)
9-, R2 is CH
3(CH
2)
2-, R3 is CH
3(CH
2)
2cH (CH
3) (CH
2)
2-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH
3(CH
2)
2-.
Be 1.44: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 32 DEG C, stratification, and the time of balancing each other is 30min; In water, lactic acid massfraction is 0.3%.
In step (d): strippant [calcium hydroxide suspension liquid] and load organic phases are mixed in pipeline reactor, after mixing, injecting reactor strips, concrete technology parameter is as shown in table 11, and [C represents the concentration of lactic acid in load organic phases, W represents the massfraction of calcium hydroxide in calcium hydroxide suspension liquid, N
1represent amount of substance hydroxy in calcium hydroxide suspension liquid, N
2represent the amount of substance of lactic acid in load organic phases]:
embodiment 12
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 24%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 6: 3: 0.8.Extraction agent is the mixture [volume ratio of the two is 1: 1] of the amides in embodiment 11 and embodiment 10, and solvent is whiteruss, and phase modifier is the mixture [volume ratio of the two is 1: 1] of the alcohol compound in embodiment 11 and embodiment 10.
Be 1.5: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 36 DEG C, stratification, and the time of balancing each other is 25min; In water, lactic acid massfraction is 0.2%.
In step (d): strippant [calcium hydroxide suspension liquid] and load organic phases are mixed in pipeline reactor, after mixing, injecting reactor strips, concrete technology parameter is as shown in table 12, and [C represents the concentration of lactic acid in load organic phases, W represents the massfraction of calcium hydroxide in calcium hydroxide suspension liquid, N
1represent amount of substance hydroxy in calcium hydroxide suspension liquid, N
2represent the amount of substance of lactic acid in load organic phases]:
In the above-described embodiments, the massfraction that heavy phase lactic acid can be diluted to lactic acid is any number between 10%-60%, extracting operation temperature can be any number between 20-70 DEG C, under similarity condition, all can realize the most lactic acid in heavy phase lactic acid are transferred to formation load organic phases in organic extraction mutually selectively, make the impurity in heavy phase lactic acid obtain effective separation with lactic acid, lactic acid massfraction in water is reduced to below 1%.The massfraction that preferably heavy phase lactic acid is diluted to lactic acid is 20%-30%, and temperature is 30-45 DEG C, can realize so better effect of extracting.
In above-described embodiment 2, embodiment 9 and embodiment 10, (CH
2)
5cH-represents that a hydrogen of hexanaphthene is substituted.
Above-described embodiment is only for the invention example is clearly described, and the not restriction to the invention embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without being also listed as thoroughly all embodiments.And the apparent variation of being extended out thus or variation are still among the protection domain in the invention claim.