CN104276967B - Method for producing low-lysine -content product - Google Patents

Method for producing low-lysine -content product Download PDF

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CN104276967B
CN104276967B CN201310273321.4A CN201310273321A CN104276967B CN 104276967 B CN104276967 B CN 104276967B CN 201310273321 A CN201310273321 A CN 201310273321A CN 104276967 B CN104276967 B CN 104276967B
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lysine
content
product
fermentation liquor
weight
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CN104276967A (en
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周勇
满云
王勇
陈静文
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Cofco Biotechnology Co Ltd
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Cofco Biochemical Anhui Co Ltd
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Abstract

The invention discloses a method for producing a low-lysine -content product. The method comprises: adjusting the pH value of a lysine fermentation liquid to be 3.5 or less, and performing solid-liquid separation to obtain a liquid phase and a dense phase both containing lysine; mixing the obtained dense phase with the lysine fermentation liquid to obtain a lysine fermentation mixed solution; and performing concentration and pelleting on the lysine fermentation mixed solution, and drying the pelleting product, so as to obtain a product particle containing lysine. The conditions for solid-liquid separation enables the volume of the dense phase to be 20-30% of the original volume of the to-be separated lysine fermentation liquid, the content of lysine in the dense phase is 10-14 wt%, and the dense phase is obtained by performing solid-liquid separation on the lysine fermentation liquid and is a phase containing more fermentation thalli compared with a clear liquid. By employing the technical scheme, the quality of the lysine salt product is improved, and energy consumption and cost are reduced.

Description

A kind of method for producing low content lysine product
Technical field
The present invention relates to a kind of method for producing low content lysine product.
Background technology
Lysine is the essential amino acids of a kind of human body and animal body, can not voluntarily be synthesized in human body and animal body, Play an important role in the metabolism of living organism, but in most of corn, lysine is the first limiting amino acids, its content It is very low, therefore, during food and feedstuff is prepared, lysine is main additive, to improve food and feedstuff in Amino acid balance, so as to promote the growth of organism.
In lysine product, actually used principal mode includes:The lysinate product of high-load and low content Lysinate product etc..
CN102442919A discloses a kind of method for producing low content lysinate product, and the method is included lysine The fermentation liquid obtained after fermentation carries out solid-liquid separation, obtains the liquid phase containing lysine and solid residue, and liquid phase is tied Crystalline substance obtains crystalline mother solution, will carry out pelletize after the solid residue for obtaining and crystalline mother solution, fermentation liquid, bentonite, Semen Maydis pulp mixing And drying prepares lysinate product.
But the method improves the ash of product while the lysinate product of low content is obtained, so as to reduce The quality of product, and the preparation method energy consumption and relatively costly.
The content of the invention
It is an object of the invention to overcome the lysinate product quality using prior art production low, and producing The shortcoming of energy consumption and high cost in journey, there is provided the production that one kind can improve lysine product quality, reducing energy consumption and cost is low The method of content lysinate product.
It was found by the inventors of the present invention that the quality of the lysine product of the low content produced using prior art is low, energy consumption And be that prior art is introduced in process of production to produce the lysinate product of low content the reason for high cost The materials such as bentonite, Semen Maydis pulp, cause the ash in lysine product to improve, so as to reduce the quality of product;Meanwhile, Semen Maydiss The addition of slurry and crystalline mother solution, increased moisture, improve the energy consumption of steam consumption and drying;In addition, carrying out to fermentation liquid solid Liquid separate when, the optimal process conditions of optimization due to the inhibition not according to fermentation thalli so that separate exist compared with Big inhibition, also increases energy consumption.
The present inventor is found surprisingly that, before lysine fermentation liquor is carried out into solid-liquid separation by its pH value adjust to Less than 3.5, make the thalline degeneration in fermentation liquid, can be effectively in separation process reduce the resistance flowed out to fermentation clear liquid of thalline Hinder effect such that it is able to reducing energy consumption;Present inventor have further discovered that simultaneously, when the volume of solid-liquid separation to concentrated phase reaches institute During the 20-30% of detached lysine fermentation liquor original volume, separating rate is substantially reduced, and now stops separating energy consumption relatively low. And the preparation of low content lysinate product is directly carried out after concentrated phase is mixed with lysine fermentation liquor, due to without bentonite And the introducing of Semen Maydis pulp, the introducing of the grey impurity that grades is reduced, the quality of lysinate product can be effectively improved;Simultaneously because Addition without extra liquid, reduces steam consumption.
Find based on more than, the invention provides a kind of method for producing low content lysine product, wherein, the method bag Include:
The pH value of lysine fermentation liquor is adjusted to less than 3.5, and carries out solid-liquid separation, obtain the clear liquid containing lysine And concentrated phase;The condition of solid-liquid separation causes the 20- that the volume of the concentrated phase for obtaining is separated lysine fermentation liquor original volume 30%, wherein, the content of lysine is 10-14 weight % in concentrated phase;
The concentrated phase for obtaining and lysine fermentation liquor are mixed to get into fermenting lysine mixed liquor;It is mixed to the fermenting lysine Close liquid to be concentrated and pelletize, and the product after pelletize is dried, obtain the product particle containing lysine;
The concentrated phase will be obtained after lysine fermentation liquor solid-liquid separation, more containing fermentation thalli relative to clear liquid Phase.
Preferably, the pH value of lysine fermentation liquor is adjusted to 2-3.5.
Preferably, the volume ratio that concentrated phase and the lysine fermentation liquor that mixed with concentrated phase are mixed is 1:8-12.
By the above-mentioned technical proposal using the present invention, do not introduce unnecessary during due to the lysine product for producing low content Moisture and other materials, so as to improve the quality of lysine product;Simultaneously as by the pH of fermentation liquid before solid-liquid separation Value is adjusted to make thalline degeneration in the scope of the present invention, and when the volume of concentrated phase is separated lysine fermentation liquor original volume Stop separating during 20-30%, effectively prevent the energy consumption that the inhibition of thalline is brought, therefore, significantly reduce and produced Energy consumption and cost in journey.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Specific embodiment
The specific embodiment of the present invention is described in detail below.It should be appreciated that described herein concrete Embodiment is merely to illustrate and explains the present invention, is not limited to the present invention.
The invention provides a kind of method that low energy consumption produces low content lysine product, wherein, the method includes:
The pH value of lysine fermentation liquor is adjusted to less than 3.5, and carries out solid-liquid separation, obtain the liquid phase containing lysine And concentrated phase;The condition of solid-liquid separation causes the 20- that the volume of the concentrated phase for obtaining is separated lysine fermentation liquor original volume 30%, wherein, the content of lysine is 10-14 weight % in concentrated phase;
The concentrated phase for obtaining and lysine fermentation liquor are carried out being mixed to get fermenting lysine mixed liquor;The lysine is sent out Ferment mixed liquor is concentrated and pelletize, and is dried to granulated, obtains the product particle containing lysine;
The concentrated phase will be obtained after lysine fermentation liquor solid-liquid separation, more containing fermentation thalli relative to clear liquid Phase.
Under normal circumstances, fermenting lysine terminates the pH of after fermentation liquid and is typically maintained in 6.5-7.1, now fermenting lysine The activity of strain is still higher, while exist between thalline interact, and thalline is more loose, the volume occupied in fermentation liquid Larger, when the fermentation liquid after directly is terminated fermenting lysine carries out solid-liquid separation, it can produce serious to solid-liquid separation Inhibition, causes solid-liquid separation to be difficult to.In this case, can only be pre- to reach to increase disengaging time and peeling strength The separation purpose of phase, but the utilization rate of equipment is so not only reduced, while also increasing power consumption.The present inventor sends out It is existing, can pass through to adjust the pH value of fermentation liquid so that the fermentation thalli degeneration in lysine fermentation liquor is even inactivated, such that it is able to Thalline is effectively reduced to detached inhibition, and then preferable separating effect can be reached.Therefore, by lysine fermentation liquor PH value is adjusted to less than 3.5;Under preferable case, the pH value of lysine fermentation liquor is adjusted to 2-3.5.
According to the present invention, the species that acid used when pH value is adjusted is carried out to lysine fermentation liquor has no particular limits.Example Such as, it is possible to use sulphuric acid and/or hydrochloric acid are adjusted to the pH value of lysine fermentation liquor.In addition, not having to the concentration of the acid yet Have special requirement, if ensure using it is described it is sour after the pH value of lysine fermentation liquor can be adjusted to above-mentioned preferred pH value model In enclosing, under preferable case, increase evaporation and consume energy to not cause to dilute to lysine fermentation liquor, the sulphuric acid for using it is dense Spend for 85-98 weight %;The concentration of the hydrochloric acid for using is 30-32 weight %.
According to the present invention, in order to further make fermentation thalli degeneration and inactivate, while the viscosity of fermentation liquid is reduced, preferably , the method is additionally included in before solid-liquid separation and the lysine fermentation liquor is heated.It was found by the inventors of the present invention that relying Propylhomoserin its stability when pH is relatively low increases, and at lower ph to lysine fermentation liquor heating, can be more preferable Make fermentation thalli degeneration therein and inactivate.Therefore, it is right and before solid-liquid separation it is highly preferred that after pH value is adjusted The lysine fermentation liquor is heated, and the temperature for being heated to the lysine fermentation liquor is 70-90 DEG C, and maintains 40- 120min.The mode of the heating is not particularly limited, and can be plate type heat exchanger heat exchange, steam jacket heating etc. for example.
Under normal circumstances, with the carrying out of lysine fermentation liquor solid-liquid separation, due to the impurity in lysine fermentation liquor with And the inhibition of fermented bacterium, the fractional dose and separating rate of fermentation clear liquid will be less and less.It was found by the inventors of the present invention that When the volume of solid-liquid separation to concentrated phase reaches the 20-30% of separated fermentation liquid original volume, the fractional dose of fermentation clear liquid is obvious Reduce, now, if continuing to separate, on the one hand need the relatively long time, on the other hand, power consumption relative increase.Therefore, root According to the present invention, when the volume of solid-liquid separation to concentrated phase reaches the 20-30% of separated fermentation liquid original volume, stop separating, this When time for consuming and energy consumption it is relatively low.Now the content of lysine is 10-14 weight % in gained concentrated phase, and thalline content is 3-6 weight %.
It is people in the art by the method that the fermentation liquid obtained after fermenting lysine carries out solid-liquid separation according to the present invention Well known to member, for example, membrance separation, disk plate centrifuge are separated etc., so as to obtain the above-mentioned clear liquid containing lysine and concentrated phase.
In this area, the lysinate product of low content generally includes the lysine product of 65 weight %(The content of lysine More than 52 weight %), 70 weight % lysine product(The content of lysine is more than 56 weight %), 75 weight % lysine Product(The content of lysine is more than 60 weight %).
According to the present invention, the concentrated phase for obtaining and lysine fermentation liquor are carried out being mixed to get fermenting lysine mixed liquor, its In, the volume ratio that concentrated phase and the lysine fermentation liquor mixed with concentrated phase are mixed can be selected in relative broad range, only Ensure that and obtain lysinate product as above, and meet the standard described in table 1.In the present invention, with institute State the lysine fermentation liquor that concentrated phase mixed and refer to the lysine fermentation liquor that fermenting lysine is adjusted after terminating without pH value.
It is to improve the stability of final gained lysinate product according to the present invention, and reduces it in storage Hygroscopicity, it is 4-6 to need to adjust its pH value before to fermenting lysine mixed liquor concentration.
The present inventor is found surprisingly that, it is of the invention it is a kind of preferred embodiment, by fermenting lysine The pH value of liquid is adjusted to 2-3.5, and by its solid-liquid separation until the volume of concentrated phase is separated lysine fermentation liquor substance The volume ratio of long-pending 20-30%, concentrated phase and the lysine fermentation liquor mixed with concentrated phase is 1:During 8-12, the lysine of gained Fermentation mixed liquor pH value just at 4-6, therefore, eliminate regulation its pH value the step of, and thus mixed fermentation liquid prepare Lysine product be the lysine product of 75 weight %.Using the preferred scheme, operating procedure is on the one hand simplified, separately On the one hand, due to being no longer adjusted to the pH value of mixed fermentation liquid, therefore, the introducing of extra water is reduce further, from And reduce further evaporation power consumption.Therefore, the volume of concentrated phase and the lysine fermentation liquor mixed with concentrated phase is preferably 1: 8-12, that is, the lysinate product of low content described herein is preferably the lysine product of 75 weight %.
According to the present invention, the lysine fermentation liquor for solid-liquid separation or the lysine for being mixed with concentrated phase are sent out The preparation method of zymotic fluid is known to those skilled in the art, to refer to and contain lysine after fermenting obtained in the method by fermenting Fermentation liquid, wherein, the content of lysine can change in very large range in the lysine fermentation liquor, and this can be according to tool The fermentation condition of body is adjusted, it is also possible to be adjusted by the mode such as concentration or dilution after fermentation ends, preferable case Under, the content of lysine can be 11-15 weight %, more preferably 12-14 weight % in the lysine fermentation liquor.
According to the present invention, the content of the lysine in the content and concentrated phase of the lysine in lysine fermentation liquor is carried out Method for measuring is known to those skilled in the art, it is, for example possible to use ninhydrin colorimetry.
According to the present invention, the energy consumption of pelletize and drying after concentration, and time and the energy consumption of concentration are taken into full account, preferably Ground, the content of lysine is 35-50 weight % in gained concentrated solution after concentration, and the content of thalline is 3-5 weight %.
Wherein, the method and condition of the concentration are known to those skilled in the art, and for example, concentration can be dense for quadruple effect Contract, the concentration condition is:One effect vapor (steam) temperature can be 85-95 DEG C, the vacuum of separation chamber can for 0.03 to 0.05MPa;Two effect vapor (steam) temperatures can be 75-90 DEG C, and the vacuum of separation chamber can be 0.050 to 0.065MPa;Triple effect steams Stripping temperature can be 65-85 DEG C, and the vacuum of separation chamber can be 0.065 to 0.08MPa;Quadruple effect vapor (steam) temperature can be 50- 75 DEG C, the vacuum of separation chamber can be 0.08 to 0.092MPa.Wherein, the vacuum is to represent system pressure actual number The strong numerical value of value subatmospheric, i.e.,:Vacuum=(Atmospheric pressure-absolute pressure).
Pelletize can be spray granulation, and the condition of the pelletize can include:The inlet temperature of pelletize is 140-190 DEG C, the pressure of air intake is 3000-4000 handkerchiefs, and leaving air temp is 70-90 DEG C, goes out wind pressure for 1500-2500 handkerchiefs.
Additionally, to the granulated condition being dried, so as to get the product particle containing lysine sulfate contain The water yield≤3 weight %(Lysine sulfate product).The lysine sulfate product for obtaining meets the requirement of table 1.
Table 1
Index name Index
1B(In terms of butt), weight % ≥60
Loss on drying, weight % ≤3.0
Ammonium salt(With NH4 +Meter), weight % ≤1.0
The discriminating of sulfate radical White precipitate
Ignition residue, weight % ≤4.0
Heavy metal(In terms of Pb), mg/kg ≤20
Arsenic(In terms of As), mg/kg ≤3
PH value 4.0-6.0
Granularity(12-30 mesh), weight % ≥90
According to the industry unified standard of lysine content detection in lysine product, no matter prepared lysine product is Sulfate product or hydrochloric acid product salt, or other types of lysinate product, determine lysine content when with The assay method of the hydrochlorate of lysine is standard, determines the lysine content in lysinate product.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment Detail, the present invention range of the technology design in, various simple variants can be carried out to technical scheme, this A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance In the case of shield, can be combined by any suitable means.In order to avoid unnecessary repetition, the present invention to it is various can The compound mode of energy is no longer separately illustrated.
Additionally, combination in any can also be carried out between a variety of embodiments of the present invention, as long as it is without prejudice to this The thought of invention, it should equally be considered as content disclosed in this invention.
In following examples and comparative example, the L- in lysine sulfate product in terms of butt is determined as follows and relies ammonia The content of acid.
(1)The preparation of 1,2,3-indantrione monohydrate chromophoric solution:
Weigh 1,2,3-indantrione monohydrate 10g, copper chloride(CuCl2·2H2O)In 1000ml volumetric flasks, then adding citric acid delays 13.4g Rush liquid 125ml(Anhydrous citric acid content is 4.24g/100ml, and sodium hydrate content is 1.68g/100ml, pH value 1.3), then add Enter 375ml ethylene glycol monomethyl ether, be then settled to 1000ml with distilled water, shake up, deposit refrigerator(5℃)Lucifuge, it is standby.
(2)The preparation of L-lysine hydrochloride standard working solution
L-lysine hydrochloride standard substance are dried to constant weight at 100 DEG C -105 DEG C, is then matched somebody with somebody respectively using distilled water Concentration processed is followed successively by the L- of 0.00mg/mL, 0.20mg/mL, 0.25mg/mL, 0.30mg/mL, 0.35mg/mL, 0.40mg/mL and relies Propylhomoserin hydrochlorate standard substance working solution.
(3)The measure of the content of the 1B in sample in terms of butt
L-lysine hydrochloride standard working solution and the sample after dilution are drawn respectively(Refer to lysine sulfate to be measured Sample)1mL is in the 25ml color comparison tubes of 7 cleanings, then draws 1mL steps respectively(1)The 1,2,3-indantrione monohydrate chromophoric solution of middle preparation is arrived In each color comparison tube, stopper is covered, wherein, the extension rate of sample causes the absorbance of sample between above-mentioned standard working solution Between the maximum and minima of absorbance.
By above-mentioned sample(Testing sample)Heat 15 minutes in boiling water with L-lysine hydrochloride standard substance, divide again after cooling Not Jia Ru 10m distilled water, after mix homogeneously, the L-lysine hydrochloride standard working solution using content as 0.00mg/mL is used as ginseng Than determining the absorbance of each solution under 480nm.
As vertical coordinate, corresponding absorbance is abscissa to concentration with L-lysine hydrochloride standard working solution, makes mark Directrix curve, draws equation of linear regression.The absorbance of institute's test sample product is substituted into equation of linear regression and tried to achieve in sample and is relied according to L- The quality of the lysine sulfate that propylhomoserin hydrochloric acid salt formation is determined, and the 1B being calculated as follows in sample in terms of butt Content.
Wherein:X:1B content, in terms of butt;
m1:The quality of L-lysine hydrochloride in institute's test sample product(mg);
n:Sample solution extension rate;
k:Conversion coefficient(0.8004);
m2:Sample quality(g);
w:Sample moisture.
Embodiment 1
The present embodiment is used to illustrate the method that the low energy consumption of present invention offer prepares the lysinate product of low content.
(1)Take 100m3The lysine fermentation liquor obtained after fermentation, wherein, the content of lysine is 13.2 weights in fermentation liquid Amount %, concentration is that the sulphuric acid of 98 weight % adjusts the pH value of the lysine fermentation liquor to 3.0, is heated to 80 DEG C.Then make Use disk plate centrifuge(GEA Westfalia Separator China, model NA7)Lysine fermentation liquor after to adjusting pH value Solid-liquid separation is carried out, the condition of solid-liquid separation is:Separation factor is 2400,75 DEG C of temperature.When the volume of solid-liquid separation to concentrated phase For separated lysine fermentation liquor original volume 20% when stop solid-liquid separation.
(2)Using ninhydrin colorimetry measuring process(1)The content of lysine is 10.9 weight % in middle gained concentrated phase.
(3)By step(1)In the concentrated phase that obtains and the lysine fermentation liquor that content is 13.5 weight % be by volume 1:10 Mixed, obtained fermenting lysine mixed liquor.The pH value of the fermenting lysine mixed liquor is 5.4.
(4)By step(3)In obtain adjust pH value after fermenting lysine mixed liquor be incorporated in four-effect evaporator Row concentration, wherein, an effect vapor (steam) temperature is 90 DEG C, separation chamber's vacuum 0.035MPa;Two 80 DEG C of vapor (steam) temperatures of effect, separation chamber is true Reciprocal of duty cycle 0.050MPa;70 DEG C of triple effect vapor (steam) temperature, separation chamber's vacuum 0.065MPa;55 DEG C of quadruple effect vapor (steam) temperature, separation chamber is true Reciprocal of duty cycle 0.08MPa, after concentration, the content of lysine is 45 weight % in the concentrated solution containing lysine, and the content of thalline is 4.5 weight %.
(5)By step(4)In the concentrated solution containing lysine that obtains be incorporated into pelletize in comminutor, the temperature of pelletize hot blast Spend for 150 DEG C, the pressure of pelletize wind is 3500 handkerchiefs, and exhaust temperature is 80 DEG C, and tail gas pressure is 2000 handkerchiefs.And draw granulated Enter to drying bed, it is 93 DEG C to be dried inlet temperature, water content≤3 weight % of the lysine sulfate granule for obtaining, i.e. rely ammonia Sour sulfate product A1.
Steam consumption and electric energy consumption in record whole process, and determine the L- in lysine sulfate product in terms of butt The content of lysine, the results are shown in Table 2.
Embodiment 2
The present embodiment is used to illustrate the method that the low energy consumption of present invention offer prepares the lysinate product of low content.
(1)Take 100m3The lysine fermentation liquor obtained after fermentation, wherein, the content of lysine is 13.2 weights in fermentation liquid Amount %, concentration is that the sulphuric acid of 85 weight % adjusts the pH value of the lysine fermentation liquor to 2.0, is heated to 90 DEG C.Then make Use disk plate centrifuge(GEA Westfalia Separator China, model NA7)Lysine fermentation liquor after to adjusting pH value Solid-liquid separation is carried out, the condition of solid-liquid separation is:Separation factor is 2400,75 DEG C of temperature.When the volume of solid-liquid separation to concentrated phase For separated lysine fermentation liquor original volume 25% when stop solid-liquid separation.
(2)Using ninhydrin colorimetry measuring process(1)The content of lysine is 12.3 weight % in middle gained concentrated phase.
(3)By step(1)In the concentrated phase that obtains and the lysine fermentation liquor that content is 13.4 weight % be by volume 1:12 Mixed, obtained fermenting lysine mixed liquor.The pH value of the fermenting lysine mixed liquor is 4.2.
(4)By step(3)In obtain adjust pH value after fermenting lysine mixed liquor be incorporated in four-effect evaporator Row concentration, wherein, an effect vapor (steam) temperature is 90 DEG C, separation chamber's vacuum 0.035MPa;Two 80 DEG C of vapor (steam) temperatures of effect, separation chamber is true Reciprocal of duty cycle 0.050MPa;70 DEG C of triple effect vapor (steam) temperature, separation chamber's vacuum 0.065MPa;55 DEG C of quadruple effect vapor (steam) temperature, separation chamber is true Reciprocal of duty cycle 0.08MPa, after concentration, the content of lysine is 50 weight % in the concentrated solution containing lysine, and the content of thalline is 4.9 weight %.
(5)By step(4)In the concentrated solution containing lysine that obtains be incorporated into pelletize in comminutor, the temperature of pelletize hot blast Spend for 150 DEG C, the pressure of pelletize wind is 3500 handkerchiefs, and exhaust temperature is 80 DEG C, and tail gas pressure is 2000 handkerchiefs.And draw granulated Enter to drying bed, it is 93 DEG C to be dried inlet temperature, water content≤3 weight % of the lysine sulfate granule for obtaining, i.e. rely ammonia Sour sulfate product A2.
Steam consumption and electric energy consumption in record whole process, and determine the L- in lysine sulfate product in terms of butt The content of lysine, the results are shown in Table 2.
Embodiment 3
The present embodiment is used to illustrate the method that the low energy consumption of present invention offer prepares the lysinate product of low content.
(1)Take 100m3The lysine fermentation liquor obtained after fermentation, wherein, the content of lysine is 13.2 weights in fermentation liquid Amount %, concentration is that the sulphuric acid of 80 weight % adjusts the pH value of the lysine fermentation liquor to 3.5, is heated to 70 DEG C.Then make Use disk plate centrifuge(GEA Westfalia Separator China, model NA7)Lysine fermentation liquor after to adjusting pH value Solid-liquid separation is carried out, the condition of solid-liquid separation is:Separation factor is 2400,75 DEG C of temperature.When the volume of solid-liquid separation to concentrated phase For separated lysine fermentation liquor original volume 30% when stop solid-liquid separation.
(2)Using ninhydrin colorimetry measuring process(1)The content of lysine is 12.3 weight % in middle gained concentrated phase.
(3)By step(1)In the concentrated phase that obtains and the lysine fermentation liquor that content is 13.4 weight % be by volume 1:8 Mixed, obtained fermenting lysine mixed liquor.The pH value of the fermenting lysine mixed liquor is 5.6.
(4)By step(3)In obtain adjust pH value after fermenting lysine mixed liquor be incorporated in four-effect evaporator Row concentration, wherein, an effect vapor (steam) temperature is 90 DEG C, separation chamber's vacuum 0.035MPa;Two 80 DEG C of vapor (steam) temperatures of effect, separation chamber is true Reciprocal of duty cycle 0.050MPa;70 DEG C of triple effect vapor (steam) temperature, separation chamber's vacuum 0.065MPa;55 DEG C of quadruple effect vapor (steam) temperature, separation chamber is true Reciprocal of duty cycle 0.08MPa, after concentration, the content of lysine is 48 weight % in the concentrated solution containing lysine, and the content of thalline is 5 weight %.
(5)By step(4)In the concentrated solution containing lysine that obtains be incorporated into pelletize in comminutor, the temperature of pelletize hot blast Spend for 150 DEG C, the pressure of pelletize wind is 3500 handkerchiefs, and exhaust temperature is 80 DEG C, and tail gas pressure is 2000 handkerchiefs.And draw granulated Enter to drying bed, it is 93 DEG C to be dried inlet temperature, water content≤3 weight % of the lysine sulfate granule for obtaining, i.e. rely ammonia Sour sulfate product A3.
Steam consumption and electric energy consumption in record whole process, and determine the L- in lysine sulfate product in terms of butt The content of lysine, the results are shown in Table 2.
Embodiment 4
The present embodiment is used to illustrate the method that the low energy consumption of present invention offer prepares the lysinate product of low content.
The preparation of lysine sulfate product is carried out according to method same as Example 1, lysine sulfate product is obtained Product A4.Except for the difference that, step(1)The middle pH value for adjusting the lysine fermentation liquor is to 1.5;Step(3)In with 13.4 weight % Lysine fermentation liquor is by volume 1:10 mixed after pH be 3.4, with sodium hydroxide adjust mixed liquor pH value to 5.4, Step(2)Middle utilization ninhydrin colorimetry measuring process(1)The content of lysine is 15.6 weight % in middle gained concentrated phase.
Steam consumption and electric energy consumption in record whole process, and determine the L- in lysine sulfate product in terms of butt The content of lysine, the results are shown in Table 2.
Embodiment 5
The present embodiment is used to illustrate the method that the low energy consumption of present invention offer prepares the lysinate product of low content.
The preparation of lysine sulfate product is carried out according to method same as Example 1, lysine sulfate product is obtained Product A5.Except for the difference that, step(1)In do not heated after the pH value for adjusting the lysine fermentation liquor.
Steam consumption and electric energy consumption in record whole process, and determine the L- in lysine sulfate product in terms of butt The content of lysine, the results are shown in Table 2.
Comparative example 1
This comparative example is used to illustrate the method that prior art produces low content lysinate product.
The preparation of lysine sulfate product is carried out according to method same as Example 1, lysine sulfate product is obtained Product A6.Except for the difference that, step(1)In do not adjust the pH value of the lysine fermentation liquor, step(3)In with 13.4 weight % rely Propylhomoserin fermentation liquid is by volume 1:After 10 are mixed, it is 5.4 to cause the pH value of mixed liquor with sulfur acid for adjusting pH.
Steam consumption and electric energy consumption in record whole process, and determine the L- in lysine sulfate product in terms of butt The content of lysine, the results are shown in Table 2.
Comparative example 2
This comparative example is used to illustrate the method that prior art produces low content lysinate product.
The preparation of lysine sulfate product is carried out according to method same as Example 1, lysine sulfate product is obtained Product A7.Except for the difference that, step(3)Middle addition is mixing with the crystalline mother solution of concentrated phase identical weight, bentonite and Semen Maydis pulp Thing.
Steam consumption and electric energy consumption in record whole process, and determine the L- in lysine sulfate product in terms of butt The content of lysine, the results are shown in Table 2.
Table 2
By upper table 1 as can be seen that embodiment 1-5 is compared with comparative example 1 with 2, lysine fermentation liquor is carried out into solid-liquid point From front, its pH value is adjusted to the scope of the present invention, 20-30 weight % of solid-liquid separation to separated fermentation liquid original volume, And due to the lysinate product of low content prepared by the addition without materials such as Semen Maydis pulp, bentonite, the method for the present invention Quality be significantly improved;Simultaneously as the addition without extra liquid, and reconcile before to fermentation liquid solid-liquid separation Its pH value can significantly reduce the energy consumption in preparation process in the scope of the present invention, so as to reduce preparation cost.By embodiment 1 compares with embodiment 4, and steam power consumption is increased while the addition of sodium hydroxide increases sodium hydroxide consumption in embodiment 4.Will Embodiment 1 is compared with embodiment 5, before solid-liquid separation is carried out to lysine fermentation liquor, is adjusted and is heated after pH value, Neng Goujin One step reducing energy consumption.Therefore, using technical scheme, improve the quality of lysinate product, reduce energy consumption and Cost.Also, the lysine fermentation liquor mixed by concentrated phase and with concentrated phase mixes according to currently preferred ratio, it is not necessary to PH value is adjusted again to mixed lysine fermentation liquor, that is, saves operating procedure, further reducing energy consumption.

Claims (6)

1. it is a kind of production 75 weight % lysine products method, it is characterised in that the method includes:
The pH value of lysine fermentation liquor is adjusted to less than 3.0, and carries out solid-liquid separation, obtain the clear liquid containing lysine and dense Phase;The condition of solid-liquid separation makes the 20-30% that the volume of the concentrated phase for obtaining is separated lysine fermentation liquor original volume, its In, the content of lysine is 10-14 weight % in concentrated phase;
Only the concentrated phase for obtaining and two kinds of components of lysine fermentation liquor are mixed to get into fermenting lysine mixed liquor;To the lysine Fermentation mixed liquor is concentrated and pelletize, and the product after pelletize is dried, and obtains the product particle containing lysine;
The concentrated phase will be obtained after lysine fermentation liquor solid-liquid separation, relative to clear liquid, containing the more phase of fermentation thalli;
Wherein, the method also includes, after the pH value for adjusting the lysine fermentation liquor, before carrying out solid-liquid separation, by institute State lysine fermentation liquor and maintain 40-120min at less than 90 DEG C at 70 DEG C;
Wherein, the method also includes that the volume ratio of the lysine fermentation liquor mixed by concentrated phase and with concentrated phase is controlled 1:8- 12, so that the pH value of the fermenting lysine mixed liquor is to 4-6, the condition of the concentration makes lysine in the concentrated solution for obtaining Content be 35-50 weight %, the content of thalline is 3-5 weight %.
2. method according to claim 1, wherein, the pH value of lysine fermentation liquor is adjusted to 2 to less than 3.0.
3. method according to claim 1, wherein, thalline content is 3-6 weight % in the concentrated phase.
4. method according to claim 1, wherein, the content of lysine is 11-15 weights in the lysine fermentation liquor Amount %.
5. method according to claim 1, wherein, the method for the pelletize is spray granulation, the condition of the pelletize Including:The inlet temperature of pelletize is 140-190 DEG C, and aspiration pressure is 3000-4000 handkerchiefs, and leaving air temp is 70-90 DEG C, goes out blast Power is 1500-2500 handkerchiefs.
6. method according to claim 1 or 5, wherein, the condition that the product after pelletize is dried, so as to get contain There is water content≤3 weight % of the product particle of lysine.
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CN110885862A (en) * 2019-09-02 2020-03-17 黑龙江成福食品集团有限公司 Preparation method of L-lysine sulfate and by-product thereof
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