阅读说明：本技术 一种由甜菜制取高品质白砂糖和黄腐酸干粉的工艺 (Process for preparing high-quality white granulated sugar and fulvic acid dry powder from beet ) 是由 刘中海 肖莉 张国玉 王陈强 王贯 张兵 柴娟 陈龙 陶飞 王军宏 杨传甲 李 于 2020-12-22 设计创作，主要内容包括：本发明公开了一种由甜菜制取高品质白砂糖和黄腐酸干粉的工艺,其具体步骤如下：1)碳酸法处理糖汁：利用碳酸法,以除去甜菜糖汁中的悬浮杂质及金属离子,经两次过滤得到二清汁；2)脱钙处理：采用阳离子Na型树脂,采用单柱处理；3)层析分离：糖汁经脱钙处理,可降低溶液中的钙含量,通过层析分离系统分离得到纯化糖分和非糖分；4)浓缩、结晶：采用四段结晶纯化工艺,降低糖浆色值；经浓缩、干燥后可得到高纯度的白砂糖；非糖分经过浓缩后、干燥后可得到黄腐酸干粉；5)包装：成品包装售出。本发明基于糖汁清净工序过程中的清汁阶段,采用强阳离子树脂交换工艺,稀汁作再生液,糖汁不会被稀释,没有糖份损失,可循环使用。(The invention discloses a process for preparing high-quality white granulated sugar and fulvic acid dry powder from beet, which comprises the following specific steps: 1) treating sugar juice by a carbonic acid method: removing suspended impurities and metal ions in the beet sugar juice by a carbonic acid method, and filtering twice to obtain second clear juice; 2) decalcification treatment: adopting cation Na type resin and adopting single column treatment; 3) chromatographic separation: the sugar juice is decalcified to reduce the calcium content in the solution, and purified sugar and non-sugar are obtained by separation through a chromatographic separation system; 4) concentration and crystallization: a four-stage crystallization purification process is adopted to reduce the color value of the syrup; the white granulated sugar with high purity can be obtained after concentration and drying; concentrating the non-sugar components, and drying to obtain fulvic acid dry powder; 5) packaging: and packaging and selling the finished product. Based on the juice cleaning stage in the sugar juice cleaning process, the invention adopts a strong cation resin exchange process, and dilute juice is used as regeneration liquid, so that the sugar juice is not diluted, has no sugar loss, and can be recycled.)

1. A process for preparing high-quality white granulated sugar and fulvic acid dry powder from beet is characterized by comprising the following specific steps:

1) treating sugar juice by a carbonic acid method: removing suspended impurities and metal ions in the beet sugar juice by a carbonic acid method, and filtering twice to obtain second clear juice;

2) decalcification treatment: adopting cation Na type resin, adopting single column treatment, consisting of 2 columns, producing in one column, regenerating in one column, passing dilute juice through the single column while the other system is regenerating, producing downstream, and regenerating in countercurrent;

3) chromatographic separation: the sugar juice of beet is decalcified, can reduce the calcium content in the sugar juice, separate and get purified sugar and nonsugar through the chromatographic separation system;

4) concentration and crystallization: the syrup adopts a four-stage crystallization purification process, so that the color value of the syrup is reduced; the white granulated sugar with high purity can be obtained after concentration and drying; concentrating the non-sugar solution, and drying to obtain fulvic acid dry powder;

5) packaging: and packaging and selling the finished product.

2. The process for preparing high-quality white granulated sugar and fulvic acid dry powder from sugar beets as claimed in claim 1, wherein: the carbonic acid method in the step 1) is characterized in that a small amount of lime which is 0.5-0.8% of the weight of the beet is added into the beet exudation juice, namely pre-lime, so that colloid is condensed and organic acid calcium salt is precipitated, the lime which is 2.0-2.5% of the weight of the beet is added into the pre-lime juice after the pre-lime juice is heated, the lime is main lime, certain non-sugar in the sugar juice is decomposed, and conditions are created for carbon dioxide saturation in the later period.

3. The process for preparing high-quality white granulated sugar and fulvic acid dry powder from sugar beets as claimed in claim 1, wherein: in the step 2), dilute juice decalcification treatment is carried out by adopting cation Na type resin, and redundant calcium ions in the sugar juice after the treatment by a carbonic acid method are removed.

4. The process for preparing high-quality white granulated sugar and fulvic acid dry powder from sugar beets as claimed in claim 1, wherein: and in the step 2), the cation Na type resin is fed and clarified by using a leaching solution, and the diluted juice is subjected to secondary filling and filtration, wherein the syrup temperature is 80-90 ℃, the Cao content is 100-250mg/L, the suspended matter content is 40-60mg/L, and the sucrose purity is 85-95%.

5. The process for preparing high-quality white granulated sugar and fulvic acid dry powder from sugar beets as claimed in claim 1, wherein: and 2) clarifying the discharged cationic Na-type resin by using a leaching solution in the step 2), and filling the filtered dilute juice for the second time, wherein the syrup temperature is 85-97 ℃, the Cao content is 0-20mg/L, the suspended matter content is 40-60mg/L, and the purity of the sucrose is 85-95%.

Technical Field

The invention relates to a process for preparing white granulated sugar, in particular to a process for preparing high-quality white granulated sugar and fulvic acid dry powder from beet.

Background

The beet is an important sugar crop, the sugar beet provides about 40 percent of global sugar, the beet can be used for preparing sugar, can also be used for preparing fuel ethanol, extracting betaine, beet fiber, preparing pectin and the like, and is one of the most concerned dominant energy crops all over the world at present. The comprehensive utilization of the beet not only reduces the sugar production cost of the beet and changes waste into valuable, but also opens up a new resource approach. The comprehensive utilization, development and research of beet has attracted the attention and exploration of researchers at home and abroad. At present, domestic sugar factories usually adopt a carbonic acid method process to produce high-quality white granulated sugar, but the treatment of the method can cause the production of carbonic acid method filter mud, thus causing environmental pollution; the addition of excess lime results in excess of Cao in the syrup, which affects the purification of sugar and the value-added processes of the molasses downstream processes.

Disclosure of Invention

The invention aims to provide a process for preparing high-quality white granulated sugar and fulvic acid dry powder from beet, which can effectively solve the problems.

In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the invention relates to a process for preparing high-quality white granulated sugar and fulvic acid dry powder from beet, which comprises the following specific steps:

1) treating sugar juice by a carbonic acid method: removing suspended impurities and metal ions in the beet sugar juice by a carbonic acid method, and filtering twice to obtain second clear juice;

2) decalcification treatment: adopting cation Na type resin, adopting single column treatment, consisting of 2 columns, producing in one column, regenerating in one column, passing dilute juice through the single column while the other system is regenerating, producing downstream, and regenerating in countercurrent;

3) chromatographic separation: the sugar juice of beet is decalcified, can reduce the calcium content in the sugar juice, separate and get purified sugar and nonsugar through the chromatographic separation system;

4) concentration and crystallization: the syrup adopts a four-stage crystallization purification process, so that the color value of the syrup is reduced; the white granulated sugar with high purity can be obtained after concentration and drying; concentrating the non-sugar solution, and drying to obtain fulvic acid dry powder;

5) packaging: and packaging and selling the finished product.

Preferably, the carbonic acid method in the step 1) is implemented by firstly adding a small amount of lime which is 0.5-0.8% of the weight of the beet into beet exudation juice, namely pre-lime, so that colloid is condensed and organic acid calcium salt is precipitated, and adding lime which is 2.0-2.5% of the weight of the beet into the pre-lime juice after heating to form main lime, so that non-sugar in the sugar juice is decomposed, and conditions are created for later carbon dioxide saturation.

Preferably, in the step 2), dilute juice decalcification treatment is performed by using a cationic Na-type resin, and excessive calcium ions in the sugar juice treated by a carbonation method are removed.

Preferably, the cationic Na-type resin feed in the step 2) is clarified by using the leaching liquor and is filled with the filtered dilute juice for the second time, the temperature of the syrup is 80-90 ℃, the Cao content is 100-250mg/L, the amount of the suspension is 40-60mg/L, and the purity of the cane sugar is 85-95%.

Preferably, the discharging of the cationic Na-type resin in the step 2) is clarified by using a leaching solution, and the diluted juice is subjected to secondary filling and filtering, wherein the temperature of syrup is 85-97 ℃, the Cao content is 0-20mg/L, the amount of a suspension is 40-60mg/L, and the purity of cane sugar is 85-95%.

Compared with the prior art, the invention has the advantages that: based on the juice cleaning stage in the sugar juice cleaning process, the invention adopts a strong cation resin exchange process, and dilute juice is used as regeneration liquid, so that the sugar juice is not diluted, has no sugar loss and can be recycled; the process provided by the invention has the advantages that the removal rate of calcium ions in the dilute juice reaches more than 90%, the softened sugar juice with good quality is provided for the production of downstream sugar and molasses, the downstream process value increment of sugar and molasses is realized, the sugar juice is not diluted in the decalcification process, and the zero discharge of wastewater is realized.

Drawings

FIG. 1 is a process flow diagram of the present invention;

FIG. 2 is a process flow of the dilute juice decalcification process of the present invention.

FIG. 3 is a flow chart of the carbonation process for sugar juice according to the present invention;

Detailed Description

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

Referring to fig. 1, 2 and 3, the process for preparing high-quality white granulated sugar and fulvic acid dry powder from sugar beets comprises the following specific steps:

1) treating sugar juice by a carbonic acid method: removing suspended impurities and metal ions in the beet sugar juice by a carbonic acid method, and filtering twice to obtain second clear juice;

2) decalcification treatment: adopting cation Na type resin, adopting single column treatment, consisting of 2 columns, producing in one column, regenerating in one column, passing dilute juice through the single column while the other system is regenerating, producing downstream, and regenerating in countercurrent;

3) chromatographic separation: the sugar juice of beet is decalcified, can reduce the calcium content in the sugar juice, separate and get purified sugar and nonsugar through the chromatographic separation system;

4) concentration and crystallization: the syrup adopts a four-stage crystallization purification process, so that the color value of the syrup is reduced; the white granulated sugar with high purity can be obtained after concentration and drying; concentrating the non-sugar solution, and drying to obtain fulvic acid dry powder;

5) packaging: and packaging and selling the finished product.

The carbonic acid method in the step 1) is characterized in that firstly, a small amount of lime which is 0.5-0.8% of the weight of the beet is added into beet exudation juice, namely pre-lime, so that colloid is condensed and organic acid calcium salt is precipitated, lime which is 2.0-2.5% of the weight of the beet is added into the pre-lime juice after the pre-lime juice is heated, the lime is main lime, non-sugar in sugar juice is decomposed, and conditions are created for carbon dioxide saturation in the later period; the white granulated sugar treated by the carbonation method has high quality, the generated precipitate can adsorb a plurality of organic non-sugar substances and various pigments contained in the sugar juice and precipitate together, and clear juice can be obtained by filtering, but simultaneously, a large amount of lime is required to be added for treatment, so that a large amount of calcium ions are left in the filtrate, which can affect the beet sugar production process, the production efficiency and the purity quality of sugar, and can affect the later extraction of the sugar component and the non-sugar component of the beet molasses by utilizing the chromatographic technique; and in the step 2), the dilute juice decalcification treatment is carried out by adopting the cation Na type resin, so that redundant calcium ions of the sugar juice treated by the carbonation method can be removed, and the aims of thoroughly removing impurities and decalcification are fulfilled.

The sugar juice is treated by the carbonic acid method, suspended impurities and metal ions in the beet sugar juice are removed by the carbonic acid method, and the second clear juice is obtained by twice filtration; among them, a sulfurous acid method may be used instead of the carbonic acid method.

In the step 2), dilute juice decalcification treatment is carried out by adopting cation Na type resin, redundant calcium ions of the sugar juice treated by a carbonation method are removed, the decalcification treatment is a set of ion-based exchange process, sodium ions in the resin replace calcium ions to complete softening of the sugar juice, the regeneration of the resin is made by using the decalcified dilute juice and concentrated (50%) caustic alkali, acid regeneration is not needed, hydrolysis of sugar is not generated, and wastewater is not generated.

The decalcification treatment in the step 2) is carried out after the sugar juice is treated and filtered by a carbonic acid method to obtain second clear juice in the process of sugar juice cleaning: the cation Na type resin feed is clarified by adopting a leaching solution, and the diluted juice is subjected to secondary filling and filtration, wherein the syrup temperature is 80-90 ℃, the Cao content is 100-250mg/L, the suspension content is 40-60mg/L, and the sucrose purity is 85-95%.

The decalcification treatment in the step 2) is carried out after the sugar juice is treated and filtered by a carbonic acid method to obtain second clear juice in the process of sugar juice cleaning: discharging the cation Na type resin, clarifying by using a leaching solution, filling the leached solution for the second time with the filtered dilute juice, wherein the temperature of the syrup is 85-97 ℃, the Cao content is 0-20mg/L, the amount of the suspension is 40-60mg/L, and the purity of the cane sugar is 85-95%.

The resin regeneration is carried out by using the softened dilute juice after decalcification, and the softened dilute juice is recycled to the upstream pre-ash or main ash process stage, so that the regeneration process has no water consumption and sugar loss and does not produce sewage.

If no dilute juice decalcification system is arranged in the early production process, the content of calcium in the beet molasses reaches 100-250mg/L, the beet molasses cannot directly enter a chromatographic analysis system, cannot be separated to obtain sugar and non-sugar, and further concentrated and dried to obtain betaine, fulvic acid dry powder and the like, and the molasses needs to enter a chromatographic separation system, a set of chemical calcium removal device is additionally arranged in the preorder of the beet molasses, so that the time and the labor are consumed, and the pollution is increased.

The color value reduction of the four-section crystallization purified syrup refers to that the crude sugar generated by one-sand crystallization in the existing three-section crystallization process of the beet processing factory is dissolved back and then enters a sand crystallization tank for crystallization and boiling, the color value of the crystallized white granulated sugar can be reduced to be within 30IU units, the national standard requirements are met, the product color value can be effectively reduced, and the equipment utilization rate is improved. The four-stage crystallization and decoloration process is technically feasible, the scheme of effectively reducing the color value of the purified syrup by the four-stage crystallization process has low investment cost, does not generate three wastes, and can realize clean production; the four-section crystallization process re-dissolves the raw sugar produced by the first sand crystallization in the existing three-section crystallization process, and then the raw sugar enters a sand crystallization tank for crystallization and boiling, and the color value of the crystallized white granulated sugar can be reduced to be within 30IU units, so that the color value meets the national standard requirement and reaches the index of qualified products. The process can realize the requirements of the four-section crystallization process by modifying the process pipeline of the existing three-section crystallization process, is convenient to modify, can effectively reduce the color value of the product, and improves the utilization rate of equipment.

Concentrating and drying: 1) purifying the syrup: after the materials enter the falling film heat exchange tube through the MVR concentration evaporation system, the materials are vaporized by heat supplied by steam, then the materials enter a steam-water separator, the material steam is compressed by a compression fan and heated and then returns to a heat exchanger, liquid is sent into the falling film tube through a circulating pump for circulating reciprocating evaporation, when the separated materials are detected to be qualified through a density meter, the materials are sent out of the system through a discharge pump, and the material brix in the process is concentrated from 30% to 65%.

MVR concentration index and running consumption of purified syrup

The evaporation capacity is 8.08 t/h;

the steam consumption is 0.06t/h, and the steam pressure is 0.3 MPa;

cooling circulation water amount of 10m³/h；

The installed capacity is 230.5 kw;

equipment investment: 512 ten thousand yuan.

2) Non-sugar residue liquid: the brix is 4.5%, the handling capacity is 67 tons/hour, the mixture is firstly concentrated from 4.5% to 9.5% by an MVR concentration system, the evaporation water amount is 35 tons/hour, the non-sugar residue amount is 31.60 tons/hour, then the mixture enters a six-effect falling film evaporation system, the brix of the residue is concentrated from 9.5% to 60%, the evaporation water amount is 26.5 tons/hour, the non-sugar residue amount is 5 tons/hour, and the concentrated non-sugar residue enters a drying system. The alcohol waste liquid enters a six-effect falling film evaporation system, is concentrated from 7 percent to 60 percent through the brix of the concentrated material, and the concentrated alcohol waste liquid is pumped to a drying system.

Non-sugar residue concentration index and consumption

The evaporation capacity is 61.5 t/h;

steam consumption is 6.7t/h, and steam pressure is 0.3 MPa;

cooling circulating water quantity of 816m³/h；

The installed capacity is 1465.5 kw;

equipment investment: 1769 ten thousand yuan.

The purified syrup concentration system adopts an MVR evaporator, and the sugar extraction residual liquid is pre-concentrated by using the MVR evaporator and then concentrated by using a multi-effect falling film evaporator.