CN105219890A - A kind of separation purification method of starch saccharificating liquid - Google Patents
A kind of separation purification method of starch saccharificating liquid Download PDFInfo
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Abstract
The invention discloses a kind of separation purification method of starch saccharificating liquid, it comprises the following steps: S1. pre-treatment: squeezed into by starch saccharificating liquid in the solid-liquid separating equipment of automatic sludge discharge and the cleaning automatically that stainless steel filtering net is housed and carry out pre-treatment; S2. ultrafiltration: pretreated feed liquid is sent in continuous ultrafiltration device and carries out continuous ultrafiltration, obtain continuous ultrafiltration liquid; S3. aftertreatment: continuous ultrafiltration liquid is through male-female ion exchange resin, concentrated, crystallization, and obtained dry concentration is β-amylose slurries or the crystal starch sugar product of 65 ~ 75%.The inventive method does not have solid waste to produce, and to the albumen reclaimed for the production of feedstuff protein, can also improve resource utilization simultaneously; Eliminate the activated carbon decolorizing operation in traditional technology, reduce consuming cost, the inventive method is simple to operate, purification effect good, energy-conserving and environment-protective, cost are low, be applicable to industrialization scale operation.
Description
Technical field
The invention belongs to technical field of membrane separation, be specifically related to a kind of separation purification method of starch saccharificating liquid.
Background technology
β-amylose is as corn with amyloid raw material, wheat, cereal, potato classes etc. are through liquefaction, saccharification, refining purification, a fluid-like state prepared by the operations such as concentrated or crystallization or crystalline product, generally comprise glucose (slurry), maltose (slurry), high fructose syrup, trehalose, Palatinose etc., wherein enzyme liquefaction and enzyme glycolysis are the committed steps of producing β-amylose, be referred to as double-enzyme method, this method mainly utilizes α-amylase (as α-amylase etc.), saccharifying enzyme is (as beta-amylase, Pullulanase, isoamylase etc.) starch molecule of long-chain is cut into micromolecular glucide, because this method has reaction conditions gentleness, Starch Conversion rate is high, the advantages such as compound decomposition reaction is few, adopted by vast β-amylose manufacturing enterprise, it is the β-amylose production technique of general practicality at present.
But because enzyme system used belongs to protein classification, simultaneously by the impact of the factor such as pH value, temperature, containing impurity such as a large amount of soluble large molecule albumen, colloid and pigments in the starch saccharificating liquid of gained, the existence of these impurity is by follow-up for severe contamination refining ion exchange resin, increase cleaning frequency and the acid and alkali consumption of resin, produce a large amount of regenerative wastewater, consume a large amount of gacs simultaneously, produce solid waste, contaminate environment, and it is high to make the energy consumption in production process, water consume, do not meet the direction of national industrial policies development.
The method that tradition removes albumen, colloid and pigment in starch saccharificating liquid has sheet frame or vacuum drum filtration method, and with diatomite as flocculating aids, improves filtration velocity, extend filtration cycle, improve the clarity of saccharification filtrate, this kind of technique, due to just using filter cloth as filtration medium, filtering accuracy is greater than 10 μm, and filtering accuracy is not high, simultaneously, because the ratio of viscosities of saccharified liquid is larger, separating effect is bad, and filtrate quality is poor, can not meet processing requirement.
Summary of the invention
The object of the invention is to the shortcoming overcoming prior art, a kind of separation purification method of starch saccharificating liquid is provided, the method is simple to operate, purification effect good, energy-conserving and environment-protective, cost are low, be applicable to industrialization scale operation.
Object of the present invention is achieved through the following technical solutions: a kind of separation purification method of starch saccharificating liquid, and it comprises the following steps:
S1. pre-treatment: squeezed into by starch saccharificating liquid in the solid-liquid separating equipment of automatic sludge discharge and the cleaning automatically that stainless steel filtering net is housed and carry out pre-treatment, the order number of described stainless steel filtering net is 100 ~ 300 orders;
S2. ultrafiltration: pretreated feed liquid sent in continuous ultrafiltration device, red-tape operati temperature is 40 ~ 70 DEG C, working pressure is 0.3 ~ 0.6MPa, cross-flow flow velocity is 5 ~ 9m/s, obtains continuous ultrafiltration liquid; Wherein, in described continuous ultrafiltration device, the aperture of film is 0.6 ~ 1.4 μm;
S3. aftertreatment: continuous ultrafiltration liquid is through male-female ion exchange resin, and to the specific conductivity≤5us/cm of effluent liquid, effluent liquid is through concentrated, crystallization, and obtained dry concentration is β-amylose slurries or the crystal starch sugar product of 65 ~ 75%.
Further, the order number of described stainless steel filtering net is 150 ~ 250 orders.
Further, in described continuous ultrafiltration device, the aperture of film is 0.8 ~ 1.2 μm.
Further, it is characterized in that, described film is polyamide membrane.
Further, the temperature of red-tape operati described in step S2 is 50 ~ 60 DEG C, working pressure is 0.4 ~ 0.5MPa, cross-flow flow velocity is 6 ~ 8m/s.
Further, described resin anion(R.A) is D301 anionite-exchange resin, and described resin cation (R.C.) is 001 × 7 Zeo-karb.
The present invention has the following advantages:
(1) automatic sludge discharge of the present invention's employing containing stainless steel filtering net and the suspension in the solid-liquid separating equipment removal starch saccharificating liquid of cleaning automatically, visible foreign, without flocculating aids, solid waste is not had to produce, to the albumen reclaimed for the production of feedstuff protein, resource utilization can also be improve simultaneously.
(2) impurity such as soluble proteins, colloid and the pigment in continuous ultrafiltration membrane separation technique removing starch saccharificating liquid are adopted, the transparence of the ultrafiltrated obtained is more than 99%, eliminate the activated carbon decolorizing operation in traditional technology, reduce consuming cost, do not have solid waste to produce.
(3) continuous ultrafiltration film impurity removal process of the present invention achieves the continuous operation of continuous feed liquor, continuously fluid, and efficiency is high, and yield can reach more than 98%.
(4) the inventive method eliminates albumen, the impurity such as colloid and pigment of in starch saccharificating liquid more than 95%, reduce the follow-up pollution to ion exchange resin, improve ion-exchange multiple, decrease regeneration of ion-exchange resin frequency, ion exchange regenerant wastewater discharge more than 80% can be reduced, save process water more than 70%, there is good water saving, energy-saving effect.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, and protection scope of the present invention is not limited to the following stated:
Embodiment 1: a kind of separation purification method of starch saccharificating liquid, it comprises the following steps:
S1. pre-treatment: starch saccharificating liquid is squeezed in the solid-liquid separating equipment of automatic sludge discharge and the cleaning automatically that stainless steel filtering net is housed and carry out pre-treatment, with remove contain in starch saccharificating liquid suspension, visible foreign, filtrate is clarified, obtains the feed liquid that transparence is 85%; The order number of described stainless steel filtering net is 100 orders;
S2. ultrafiltration: pretreated feed liquid is sent in continuous ultrafiltration device, red-tape operati temperature is 40 DEG C, working pressure is 0.3MPa, cross-flow flow velocity is 5m/s, the impurity such as albumen, colloid and pigment in further removal starch saccharificating liquid, purification starch saccharificating liquid, obtains the continuous ultrafiltration liquid that transparence is 99.4%; Wherein, in described continuous ultrafiltration device, the aperture of film is 0.6 μm of described film is polyamide membrane;
S3. aftertreatment: continuous ultrafiltration liquid is through male-female ion exchange resin, resin anion(R.A) is D301 anionite-exchange resin, and resin cation (R.C.) is 001 × 7 Zeo-karb, to the specific conductivity≤5us/cm of effluent liquid, effluent liquid is through concentrated, and obtained dry concentration is the β-amylose slurries of 65%.
Embodiment 2: a kind of separation purification method of starch saccharificating liquid, it comprises the following steps:
S1. pre-treatment: starch saccharificating liquid is squeezed in the solid-liquid separating equipment of automatic sludge discharge and the cleaning automatically that stainless steel filtering net is housed and carry out pre-treatment, with remove contain in starch saccharificating liquid suspension, visible foreign, filtrate is clarified, obtains the feed liquid that transparence is 87%; The order number of described stainless steel filtering net is 300 orders;
S2. ultrafiltration: pretreated feed liquid is sent in continuous ultrafiltration device, red-tape operati temperature is 70 DEG C, working pressure is 0.6MPa, cross-flow flow velocity is 9m/s, the impurity such as albumen, colloid and pigment in further removal starch saccharificating liquid, purification starch saccharificating liquid, obtains the continuous ultrafiltration liquid that transparence is 99.5%; Wherein, in described continuous ultrafiltration device, the aperture of film is 1.4 μm; Described film is polyamide membrane;
S3. aftertreatment: continuous ultrafiltration liquid is through male-female ion exchange resin, resin anion(R.A) is D301 anionite-exchange resin, and resin cation (R.C.) is 001 × 7 Zeo-karb, to the specific conductivity≤5us/cm of effluent liquid, effluent liquid is through concentrated, and obtained dry concentration is the β-amylose slurries of 75%.
Embodiment 3: a kind of separation purification method of starch saccharificating liquid, it comprises the following steps:
S1. pre-treatment: starch saccharificating liquid is squeezed in the solid-liquid separating equipment of automatic sludge discharge and the cleaning automatically that stainless steel filtering net is housed and carry out pre-treatment, with remove contain in starch saccharificating liquid suspension, visible foreign, filtrate is clarified, obtains the feed liquid that transparence is 84%; The order number of described stainless steel filtering net is 150 orders;
S2. ultrafiltration: pretreated feed liquid is sent in continuous ultrafiltration device, described red-tape operati temperature is 50 DEG C, working pressure is 0.4MPa, cross-flow flow velocity is 6m/s, the impurity such as albumen, colloid and pigment in further removal starch saccharificating liquid, purification starch saccharificating liquid, obtains the continuous ultrafiltration liquid that transparence is 99.3%; Wherein, in described continuous ultrafiltration device, the aperture of film is 0.8 μm; Described film is polyamide membrane;
S3. aftertreatment: continuous ultrafiltration liquid is through male-female ion exchange resin, resin anion(R.A) is D301 anionite-exchange resin, and resin cation (R.C.) is 001 × 7 Zeo-karb, to the specific conductivity≤5us/cm of effluent liquid, effluent liquid is through concentrated, and obtained dry concentration is the β-amylose slurries of 70%.
Embodiment 4: a kind of separation purification method of starch saccharificating liquid, it comprises the following steps:
S1. pre-treatment: starch saccharificating liquid is squeezed in the solid-liquid separating equipment of automatic sludge discharge and the cleaning automatically that stainless steel filtering net is housed and carry out pre-treatment, with remove contain in starch saccharificating liquid suspension, visible foreign, filtrate is clarified, obtains the feed liquid that transparence is 88%; The order number of described stainless steel filtering net is 250 orders;
S2. ultrafiltration: pretreated feed liquid is sent in continuous ultrafiltration device, described red-tape operati temperature is 60 DEG C, working pressure is 0.5MPa, cross-flow flow velocity is 8m/s, the impurity such as albumen, colloid and pigment in further removal starch saccharificating liquid, purification starch saccharificating liquid, obtains the continuous ultrafiltration liquid that transparence is 99.6%; Wherein, in described continuous ultrafiltration device, the aperture of film is 1.2 μm; Described film is polyamide membrane;
S3. aftertreatment: continuous ultrafiltration liquid is through male-female ion exchange resin, resin anion(R.A) is D301 anionite-exchange resin, and resin cation (R.C.) is 001 × 7 Zeo-karb, to the specific conductivity≤5us/cm of effluent liquid, effluent liquid is through concentrated, and obtained dry concentration is the β-amylose slurries of 72%.
Embodiment 5: a kind of separation purification method of starch saccharificating liquid, it comprises the following steps:
S1. pre-treatment: starch saccharificating liquid is squeezed in the solid-liquid separating equipment of automatic sludge discharge and the cleaning automatically that stainless steel filtering net is housed and carry out pre-treatment, with remove contain in starch saccharificating liquid suspension, visible foreign, filtrate is clarified, obtains the feed liquid that transparence is 86%; The order number of described stainless steel filtering net is 200 orders;
S2. ultrafiltration: pretreated feed liquid is sent in continuous ultrafiltration device, described red-tape operati temperature is 55 DEG C, working pressure is 0.46MPa, cross-flow flow velocity is 7m/s, the impurity such as albumen, colloid and pigment in further removal starch saccharificating liquid, purification starch saccharificating liquid, obtains the continuous ultrafiltration liquid that transparence is 99.5%; Wherein, in described continuous ultrafiltration device, the aperture of film is 1.0 μm; Described film is polyamide membrane;
S3. aftertreatment: continuous ultrafiltration liquid is through male-female ion exchange resin, resin anion(R.A) is D301 anionite-exchange resin, and resin cation (R.C.) is 001 × 7 Zeo-karb, to the specific conductivity≤5us/cm of effluent liquid, effluent liquid, through concentrated, crystallization, obtains crystal starch sugar product.
Below by way of description of test beneficial effect of the present invention:
Test example 1: the membrane pore size of continuous ultrafiltration film is on the impact of the membrane flux of starch saccharificating liquid
Test conditions: in continuous ultrafiltration membrane separation unit, red-tape operati temperature is 50 DEG C, working pressure is 0.4MPa, cross-flow flow velocity is 6m/s, and measuring the ultra-filtration membrane of different pore size affects situation to the membrane flux of starch saccharificating liquid, and test-results is in table 1.
Table 1: membrane pore size affects result to starch saccharificating liquid membrane flux
| Membrane pore size (μm) | Membrane flux (L/m 2·h) |
| 0.2 | 74.5 |
| 0.4 | 80.9 |
| 0.6 | 95.4 |
| 0.8 | 117.5 |
| 1.0 | 121.4 |
| 1.2 | 110.7 |
| 1.4 | 90.1 |
| 1.6 | 82.8 |
| 1.8 | 73.5 |
As can be seen from Table 1, along with the increase of membrane pore size, reduce again after the membrane flux of starch saccharificating liquid first increases, wherein reach maximum value when membrane pore size is 1.0 μm, this may be due to the albumen in starch saccharificating liquid, the particle diameter of the impurity such as colloid and pigment is greatly about about 1.4 μm, therefore the surface that aperture is the ultra-filtration membrane of 1.4 μm-1.8 μm can be adsorbed on, form gel coat, along with constantly carrying out of filtering, macromolecular albumen, the impurity such as colloid and pigment can cause ultra-filtration membrane hole plug, membrane flux is caused sharply to decline, and the ultra-filtration membrane that aperture is 0.2 μm-1.4 μm is far smaller than the particle diameter of impurity macromolecular substance in starch saccharificating liquid due to aperture, so these particulates can not cause Pore Blocking.Therefore in order to improve operational efficiency, and reduce investment outlay and reduce running cost, the membrane pore size of the continuous ultrafiltration film of selection controls at 0.6 μm-1.4 μm, especially 0.8 μm-1.2 μm.
Test example 2: service temperature is on the impact of starch saccharificating liquid membrane flux
Test conditions: select membrane pore size to be the ultra-filtration membrane of 1.0 μm, red-tape operati pressure is 0.4MPa, cross-flow flow velocity is 6m/s, measuring different operating temperature affects situation to starch saccharificating liquid membrane flux, and test-results is in table 2.
Table 2: service temperature affects result to starch saccharificating liquid membrane flux
| Service temperature (DEG C) | Membrane flux (L/m 2·h) |
| 20 | 75.4 |
| 30 | 79.8 |
| 40 | 91.2 |
| 50 | 104.5 |
| 60 | 108.8 |
| 70 | 112.1 |
| 80 | 114.7 |
| 90 | 116.2 |
As can be seen from Table 2, along with temperature raises, membrane flux increases thereupon, this may be due to the rising along with temperature, molecular diffusivity increases, the viscosity degradation of starch saccharificating liquid, components dissolved degree increases, therefore membrane flux improves, but find from test, if service temperature is too high, starch saccharificating liquid can be made to produce boiling taste, even there is protein denaturation, have a strong impact on the quality of saccharified liquid, and cause the wasting of resources, energy consumption raises, therefore, consider, the service temperature of continuous ultrafiltration film impurity removal process is controlled at 40-70 DEG C, preferred service temperature is 50-60 DEG C.
Test example 3: working pressure is on the impact of starch saccharificating liquid membrane flux
Test conditions: select membrane pore size to be the ultra-filtration membrane of 1.0 μm, red-tape operati temperature is 50 DEG C, cross-flow flow velocity is 6m/s, measuring different operating pressure affects situation to starch saccharificating liquid membrane flux, and test-results is in table 3.
Table 3: working pressure affects result to starch saccharificating liquid membrane flux
| Working pressure (MPa) | Membrane flux (L/m 2·h) |
| 0.2 | 82.3 |
| 0.3 | 95.7 |
| 0.4 | 112.5 |
| 0.5 | 110.3 |
| 0.6 | 101.7 |
| 0.7 | 88.3 |
As can be seen from Table 3, along with the increase of working pressure, the membrane flux of starch saccharificating liquid increases thereupon, but this trend is not linear, when pressure increase is to 0.4MPa, membrane flux change reduces, this may be because pressure is when below 0.4MPa, the dedoping step of continuous ultrafiltration film is mainly stressed control, but after pressure raises, ultrafiltration membrane surface absorption and sedimental subsidence rate increase, and the shearing force be greater than during starch saccharificating liquid cross-flow face, Pore Blocking and face concentration polarization cause pollution speed to be accelerated, therefore, consider energy consumption and filter effect, the working pressure of continuous ultrafiltration film impurity removal process is controlled at 0.3-0.6MPa, preferred working pressure is 0.4-0.5MPa.
Test example 4: cross-flow flow velocity is on the impact of starch saccharificating liquid membrane flux
Test conditions: select membrane pore size to be the ultra-filtration membrane of 1.0 μm, red-tape operati temperature is 50 DEG C, working pressure is 0.4MPa, measuring cross-flow flow velocity affects situation to starch saccharificating liquid membrane flux, and test-results is in table 4.
Table 4: cross-flow flow velocity affects result to starch saccharificating liquid membrane flux
| Cross-flow flow velocity (m/s) | Membrane flux (L/m 2·h) |
| 4 | 152.8 |
| 5 | 189.5 |
| 6 | 227.2 |
| 7 | 215.9 |
| 8 | 208.4 |
| 9 | 196.7 |
| 10 | 175.6 |
As can be seen from Table 4, along with increasing of cross-flow flow velocity, membrane flux raises gradually, this may be because flow velocity increases, starch saccharificating liquid increases the shearing force of ultra-filtration membrane settled layer, thus make the corresponding increase of membrane flux, and when cross-flow flow velocity reaches 6m/s, membrane flux reaches maximum value, then reduce gradually again, this may be owing to increasing flow velocity simply, the absorption of ultrafiltration face is constantly superposed with throw out, after saturated, shearing force and the sedimentary adsorptive power of starch saccharificating liquid tend to balance, then, balance is destroyed, flux depression.Generally, cross-flow flow velocity is too little, and ultra-filtration membrane is easily polluted; Cross-flow flow velocity is too high, has not only consumed energy but also has been unfavorable for the increase of membrane flux.Therefore, select the cross-flow flow velocity of 5-9m/s more suitable, preferred cross-flow flow velocity is 6-8m/s.
Claims (6)
1. a separation purification method for starch saccharificating liquid, is characterized in that, it comprises the following steps:
S1. pre-treatment: squeezed into by starch saccharificating liquid in the solid-liquid separating equipment of automatic sludge discharge and the cleaning automatically that stainless steel filtering net is housed and carry out pre-treatment, the order number of described stainless steel filtering net is 100 ~ 300 orders;
S2. ultrafiltration: pretreated feed liquid sent in continuous ultrafiltration device, red-tape operati temperature is 40 ~ 70 DEG C, working pressure is 0.3 ~ 0.6MPa, cross-flow flow velocity is 5 ~ 9m/s, obtains continuous ultrafiltration liquid; Wherein, in described continuous ultrafiltration device, the aperture of film is 0.6 ~ 1.4 μm;
S3. aftertreatment: continuous ultrafiltration liquid is through male-female ion exchange resin, and to the specific conductivity≤5us/cm of effluent liquid, effluent liquid is through concentrated, crystallization, and obtained dry concentration is β-amylose slurries or the crystal starch sugar product of 65 ~ 75%.
2. the separation purification method of a kind of starch saccharificating liquid as claimed in claim 1, is characterized in that, the order number of described stainless steel filtering net is 150 ~ 250 orders.
3. the separation purification method of a kind of starch saccharificating liquid as claimed in claim 1, is characterized in that, in described continuous ultrafiltration device, the aperture of film is 0.8 ~ 1.2 μm.
4. the separation purification method of a kind of starch saccharificating liquid as described in claim 1 or 3, is characterized in that, described film is polyamide membrane.
5. the separation purification method of a kind of starch saccharificating liquid as claimed in claim 1, is characterized in that, the temperature of red-tape operati described in step S2 is 50 ~ 60 DEG C, working pressure is 0.4 ~ 0.5MPa, cross-flow flow velocity is 6 ~ 8m/s.
6. the separation purification method of a kind of starch saccharificating liquid as claimed in claim 1, is characterized in that, described resin anion(R.A) is D301 anionite-exchange resin, and described resin cation (R.C.) is 001 × 7 Zeo-karb.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106512739A (en) * | 2016-09-24 | 2017-03-22 | 合肥信达膜科技有限公司 | Membrane separation method for purification of starch saccharification liquid |
| CN115055168A (en) * | 2022-06-09 | 2022-09-16 | 珠海高新区维得力生物工程有限公司 | Preparation process applied to fructo-oligosaccharide chromatographic separation filler and artificial intelligence separation device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115055168B (en) * | 2022-06-09 | 2023-05-26 | 珠海高新区维得力生物工程有限公司 | Preparation process applied to fructo-oligosaccharide chromatographic separation filler and artificial intelligent separation device |
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