阅读说明：本技术 一种用于甜菜制糖糖分高效分离方法 (Efficient separation method for sugar in sugar production of beet ) 是由 肖莉 刘中海 张国玉 王陈强 王贯 张兵 柴娟 陈龙 陶飞 王军宏 杨传甲 李 于 2020-12-15 设计创作，主要内容包括：本发明公开了一种用于甜菜制糖糖分高效分离方法,其具体步骤包括糖蜜预处理、层析分离、浓缩结晶、糖量检测；1)糖蜜预处理：糖蜜加热到70-90℃,用洗提水稀释至50-70%,稀释后的糖蜜水溶液,去除悬浮杂质,经过滤得到不含悬浮杂质和钙、镁等的清净汁液；2)层析分离：顺序式模拟移动床,分离得到两项,提取相含有高回收率的蔗糖,残液相含有高回收率的非糖；3)浓缩结晶：蒸发浓缩至65-75%锤度,存储,经4段煮糖结晶,得到合格白砂糖(色值≤35IU),提取相浓缩结晶获得纯化糖浆蔗糖纯度可达到89-95%,锤度为30-35～0Bx,糖分回收率为88-95%；4)糖量检测：用高效液相色谱检测蔗糖纯度。本发明设计合理,使用环保,经济效益高,能够获得高纯度组分。(The invention discloses a high-efficiency separation method for sugar in sugar production of beet, which comprises the specific steps of molasses pretreatment, chromatographic separation, concentration and crystallization, and sugar amount detection; 1) pretreatment of molasses: heating molasses to 70-90 deg.C, diluting with eluting water to 50-70%, removing suspended impurities from diluted molasses water solution, and filtering to obtain clean juice containing no suspended impurities and calcium, magnesium, etc.; 2) chromatographic separation: separating two items by a sequential simulated moving bed, wherein an extraction phase contains cane sugar with high recovery rate, and a residual liquid phase contains non-sugar with high recovery rate; 3) concentration and crystallization: evaporating and concentrating to 65-75% of brix, storing, decocting and crystallizing for 4 stages to obtain qualified white sugar (color value is less than or equal to 35 IU), concentrating and crystallizing the extract phase to obtain purified productThe purity of syrup sucrose can reach 89-95%, and the brix is 30-35 0 Bx, the sugar recovery rate is 88-95%; 4) and (3) sugar content detection: the purity of the sucrose was checked by high performance liquid chromatography. The invention has reasonable design, environmental protection in use and high economic benefit, and can obtain high-purity components.)

1. A high-efficiency separation method for sugar in sugar production of beet is characterized in that the method comprises the specific steps of molasses pretreatment, chromatographic separation, concentration and crystallization, and sugar amount detection;

1) pretreatment of molasses: heating molasses to 70-90 deg.C, diluting with eluting water to 50-70%, filtering the diluted molasses water solution with plate-and-frame filter to remove suspended impurities, removing impurities such as calcium and magnesium from the molasses filtrate by chemical method or ion exchange chromatography, and filtering to obtain clean juice containing no suspended impurities and calcium and magnesium;

2) chromatographic separation: separating two items by a sequential simulated moving bed, wherein an extraction phase contains cane sugar with high recovery rate, and a residual liquid phase contains non-sugar with high recovery rate;

3) concentration and crystallization: evaporating and concentrating to 65-75% of brix, storing, decocting and crystallizing for 4 times to obtain qualified white sugar (color value is less than or equal to 35 IU), concentrating and crystallizing the extract phase to obtain purified syrup sucrose with purity of 89-95% and brix of 30-35%⁰Bx, the sugar recovery rate is 88-95%;

4) and (3) sugar content detection: the purity of the sucrose was checked by high performance liquid chromatography.

2. The method for efficiently separating sugar in sugar production from sugar beets according to claim 1, wherein: the washing water is deionized water or pure water.

3. The method for efficiently separating sugar in sugar production from sugar beets according to claim 1, wherein: said step 2) is a sequential simulated moving bed, a continuous chromatographic system, wherein the feed is continuously pushed to a chromatographic separation unit, and fructose and glucose/polysaccharide fractions are separately extracted; wherein the chromatography material is ion exchange resin XA2004/32Na, and the binding force of each component is different.

Technical Field

The invention relates to a separation method, in particular to a high-efficiency separation method for sugar in sugar production of beet.

Background

In recent years, the planting scale of Chinese beet is getting bigger and bigger, the amount of beet molasses is getting bigger and bigger, the technical difficulty of processing beet molasses is small, the investment is small, and the economic benefit is better. A large amount of molasses is generated in the process of preparing sugar from beet, the molasses is a part which is difficult to degrade in wastes of a sugar factory, not only seriously pollutes the environment, but also becomes a bottleneck for restricting the sustainable development of economy of the sugar factory, is a second most pollution source of paper-making waste liquid, the treatment of the molasses by the conventional biochemical method cannot meet the requirement of standard discharge of waste water at present, and the effective treatment of the molasses becomes a key for a company to continuously produce high-quality sugar. And by adopting an advanced sugar manufacturing process technology, the loss of the sugar process can be reduced, the energy is effectively saved, the emission is reduced, the sugar manufacturing industrial chain of the beet is extended, and the sustainable development of the sugar manufacturing industry of the beet is promoted by taking the benefit as the center.

Disclosure of Invention

The invention aims to provide the efficient sugar separation method for sugar production by beet, which has the advantages of reasonable design, environmental protection and high economic benefit.

In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the invention relates to a high-efficiency separation method for sugar in sugar production of beet, which comprises the specific steps of molasses pretreatment, chromatographic separation, concentration and crystallization and sugar quantity detection.

1) Pretreatment of molasses: heating molasses to 70-90 deg.C, diluting with eluting water to 50-70%, filtering the diluted molasses water solution with plate-and-frame filter to remove suspended impurities, removing impurities such as calcium and magnesium from the molasses filtrate by chemical method or ion exchange chromatography, and filtering to obtain clean juice containing no suspended impurities and calcium and magnesium;

2) chromatographic separation: separating two items by a sequential simulated moving bed, wherein an extraction phase contains cane sugar with high recovery rate, and a residual liquid phase contains non-sugar with high recovery rate;

3) concentration and crystallization: evaporating and concentrating to 65-75% of brix, storing, decocting and crystallizing for 4 times to obtain qualified white sugar (color value is less than or equal to 35 IU), concentrating and crystallizing the extract phase to obtain purified syrup sucrose with purity of 89-95% and brix of 30-35%⁰Bx, the sugar recovery rate is 88-95%;

4) and (3) sugar content detection: the purity of the sucrose was checked by high performance liquid chromatography.

Preferably, the washing water is deionized water or pure water.

Preferably, the process in step 2) is a sequential simulated moving bed, a continuous chromatography system, where the feed is continuously pushed to a chromatographic separation unit and the fructose and glucose/polysaccharide components are separately extracted. Wherein the chromatography material is ion exchange resin XA2004/32Na, and the binding force of each component is different.

Compared with the prior art, the invention has the advantages that: the invention has reasonable design, environmental protection in use and high economic benefit, can obtain high-purity components, adopts a continuous chromatography system as a process, feeds are continuously pushed to a chromatography separation unit, and fructose and glucose/polysaccharide components are respectively extracted; compared with other batch processes, the system has no extraction, mixing and re-feeding of intermediate components, and the continuous system has lower water consumption and resin consumption per unit of separation; introducing molasses at 70-90 deg.C, and diluting the molasses in chromatographic column to 50-70% concentration; dissolved gases in the feed eluent must be removed before entering the chromatographic separator; the elution water should be deionized and the demineralization required prior to feeding is satisfactory and does not require regeneration.

Drawings

FIG. 1 is a material balance diagram of the present invention;

FIG. 2 is a diagram of the process flow (including material balance) of the present invention;

FIG. 3 is a process flow diagram of a chromatographic desugaring system.

Detailed Description

The invention will be further explained with reference to the drawings.

The invention relates to a high-efficiency separation method for sugar in sugar production of beet, which comprises the specific steps of molasses pretreatment, chromatographic separation, concentration and crystallization, and sugar amount detection;

1) pretreatment of molasses: heating molasses to 70-90 deg.C, diluting with eluting water to 50-70%, filtering the diluted molasses water solution with plate-and-frame filter to remove suspended impurities, removing impurities such as calcium and magnesium from the molasses filtrate by chemical method or ion exchange chromatography, and filtering to obtain clean juice containing no suspended impurities and calcium and magnesium;

2) chromatographic separation: separating two items by a sequential simulated moving bed, wherein an extraction phase contains cane sugar with high recovery rate, and a residual liquid phase contains non-sugar with high recovery rate;

3) concentration and crystallization: evaporating and concentrating to 65-75% of brix, storing, and crystallizing by boiling for 4 times to obtain qualified white sugar (color value is less than or equal to 35I)U), concentrating and crystallizing the extract phase to obtain purified syrup sucrose with purity of 89-95% and brix of 30-35%⁰Bx, the sugar recovery rate is 88-95%;

4) and (3) sugar content detection: the purity of the sucrose was checked by high performance liquid chromatography.

The washing water is deionized water or pure water.

The process in step 2) is a sequential simulated moving bed, a continuous chromatography system where the feed is continuously pushed to a chromatographic separation unit and the fructose and glucose/polysaccharide fractions are separately extracted. Wherein the chromatography material is ion exchange resin XA2004/32Na, and the binding force of each component is different.

Examples

After the beet production is stopped in the squeezing period, the chromatographic desugaring equipment is continuously utilized to extract the syrup to produce the white granulated sugar, but the calcium content in the molasses is far beyond the feeding requirement of the chromatographic separation system, so when the molasses is treated, the calcium ion concentration in the molasses must be reduced by adopting a chemical softening method, and then the chromatographic separation system is adopted.

Chemical calcium-removing process

Referring to the material balance diagram of fig. 1, beet molasses is stored in a molasses storage tank, pumped to a chemical decalcification unit by a molasses pump, and diluted to obtain molasses with a brix of 80⁰Bx is reduced to 50-70⁰Bx, adding sodium carbonate to soften, forming calcium carbonate precipitate, then filtering by a plate frame filter and a candle filter, wherein impurities such as suspended matters, calcium carbonate precipitate and the like are discharged in the form of filter mud, the softened molasses enters a chromatographic separation unit to extract syrup after being degassed, the molasses chemical calcium removal equipment mainly comprises a molasses dilution tank, a softening reaction tank, a plate frame filter, a candle filter and the like, the process flow is complex, and wastes such as filter mud and the like are discharged.

Chromatographic separation system

The invention relates to a set of chromatographic separation system, the equipment has the production capacity of processing 225 tons of molasses (softened molasses) every day, the purity of the separated purified syrup cane sugar can reach 89-95%, and the brix is 30-35⁰Bx, the recovery rate of sugar in molasses is 88-95%, the purity of separated residual liquid cane sugar is 10%, and brix is 4-6⁰Bx。

The chromatographic separation principle is as follows: a chromatographic separation system, named sequential simulative moving bed chromatographic desugaring system, features that the molasses is separated from other components by the different flowing speeds of its components in resin column, the molasses is adsorbed by resin while the non-sugar is not adsorbed by resin, resulting in speed difference between sugar and non-sugar, and the purified syrup with purity 89-95% and brix 30-35% is continuously collected⁰Bx, the sugar recovery rate is 88-95%. The hammer degree of the non-sugar residue is 4-6⁰Bx, containing a large amount of non-sugar and pigment.

The feed for chromatographic recovery of beet molasses is primarily characterized as follows,

type (2): beet molasses

Dry matter: 50-70% (dry basis)

The feed sucrose content: 55-65% (dry basis)

Betaine content of 4.0-6.0% (dry basis)

Non-sugar content: 24-28% (dry basis)

(Ca + Mg) divalent ion: < 500 ppm (dry basis)

Dissolved oxygen: <1ppm

Temperature: 70-90 deg.C

Suspended solids: zero

Microorganism indexes are as follows: meets the requirements of drinking water

The discharge of chromatographic recovered beet molasses is mainly characterized as follows:

type (2): purified syrup

Dry matter: 25-35% (dry basis)

The content of sucrose: 88-95% (dry basis)

Glucose content: 1.5-5.5% (dry basis)

Fructose content 0.9-1.2% (dry basis)

Type (2): non-sugar residue

PH ：7.1-8.0

Dry matter: 4.5-5.5% (dry basis)

The content of sucrose: 8.8-9.0% (dry basis)

Glucose content: 0.7-0.9% (dry basis)

Fructose content 0.8-1.0% (dry basis)

See FIG. 2 for a process flow (including material balance) chart (calculated as 225 tons molasses throughput per day)

Chromatographic separation process

Referring to the process flow diagram of the chromatographic desugaring system of fig. 3, the main body equipment is composed of 2 chromatographic columns with diameter of 4.8 m and height of 10 m, each chromatographic column is divided into 3 chambers, the total number of the two columns is 6, each chamber is provided with a circulating pump, and 1 to 6 chambers are connected in series through a pipeline and the circulating pump. The inlet end of each chamber of the chromatographic desugaring system is provided with 4 channels: the inlet and outlet of No. 1 molasses, the inlet of No. 2 condensed water, the outlet of No. 3 raffinate and the outlet of No. 4 syrup are realized according to the process requirements at each working stage.

The chromatographic system works as follows: the chromatographic separation system is an industrial application of a sequential simulated moving bed principle in a molasses sugar extraction process, and the working process of the chromatographic separation system is that 4 stages are used as 1 cycle period, and 4 stages are A: feeding and systemic circulation, B, discharging the extracting solution (simultaneously feeding purified water), C, discharging the residual liquid (simultaneously feeding molasses) and D, washing with water.

Step A: a proper amount of molasses is pumped into the chromatographic column, and air in the column must be discharged, so that the molasses is prevented from leaving blank spaces in the column due to air residue, and the pressure and material fluctuation of the chromatographic column is prevented from being influenced. And (3) after air is discharged, starting a column bottom circulating pump to start system circulation, when the circulating flux reaches a set value of a flow meter, separating sucrose components from non-sugar components, wherein a sucrose component enrichment area appears in the chamber 1, a non-sugar component enrichment area appears in the chamber 3, and the step A is finished.

B, step C: and (4) after the step A is finished, automatically switching the program to the step B and the step C, simultaneously operating the step B and the step C, feeding purified water into a chamber 1, simultaneously opening a discharging bottom valve, and ejecting the sucrose components out of the chromatography system. And step C, pumping the molasses to a feed inlet of 3 chambers, and ejecting the non-sugar components out of the chromatography system by utilizing the molasses, so that the feeding of the molasses and the discharging of the non-sugar residual liquid are realized in the link, and the system can be maintained normal.

And D, step D: after B and C end, control system automatic switch over to D step, D step is the water washing stage, sends into the pure water from 2 rooms of feed inlets, washes 2 indoor components such as inorganic salt, pigment of enrichment, ensures 2 rooms of impurity-free, guarantees next cycle period purification syrup purity, and for guaranteeing that system pressure is stable simultaneously, discharges remaining non-sugar raffinate by 3 rooms of discharge gates.

This cycle is completed by the start of the next cycle, the second cycle, 2 chambers to remove the sucrose content and 4 chambers to remove the non-sugar residue. This cycle is repeated, and sucrose components and non-sugar residual liquid are sequentially discharged from 1 to 6 chambers, so that the process is called a sequential simulated moving bed chromatographic separation technique.

The process water will be the following clean condensed water or softened filtered water, with the following indices:

dissolved solids content of maximum 0.1% w/w

Mechanical impurities no insoluble solids were detected.

Conductivity < 500. mu.S/cm

The hardness is less than or equal to 5 degrees f = 3 degrees DH

Active chloride ion 0 mg/l

Maximum dissolved oxygen of 1ppm

The lowest temperature is 85 DEG C

Maximum 0.3ppm of iron

The microorganism index accords with the index of drinking water.