JPS6230000A - Recovery of sugar from sugar stock material - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

[Detailed Description of the Invention] The present invention relates to a method for cleaning sugar solution and recovering sugar. More specifically, the present invention relates to a method for cleaning sugar solution and recovering sugar. More specifically, the present invention relates to a method for cleaning sugar solution and recovering sugar, and more specifically, a combination of ultraponic method and electrodialysis method during the production process of raw sugar from sugar cane. The present invention relates to a method for cleaning sugar solution and improving the yield of sugar products.

To explain the manufacturing process of raw sugar from cane that is currently generally carried out, cane is squeezed using a press, and mixed juice and bagasse are extracted. Next, the mixed juice is heated, milk of lime is added in a pH adjustment tank, and after rough heating, it is separated into clean juice and mud in a continuous Iti tank.

The mud is separated into r-filtrate and lime cake using a continuous negative nitrogen rotary filter, and the p-filtrate is mixed into the clean juice.The lime cake is discarded outside the manufacturing process.

Next, the purified juice is condensed in a can to obtain Shiratsu, and the Shiratsu is further roasted with sugar in a vacuum crystallizer to obtain Shiroshita. The white bottom is separated into sugar crystals (I sugar) and molasses (I molasses) by centrifugation. The molasses is further roasted and separated twice to obtain sugar crystals (II, II sugar) and molasses (1,1 molasses). The final stage of roasting sugar and the molasses obtained by separation are used as blackstrap molasses.

This method of roasting sugar and separating is called the three-stage roasting and separating method, and is the most common method.

Next, a schematic diagram of the five-stage sugar roasting/separation method is shown.

The blackstrap molasses produced from the Shirashita Sugar Factory is a molasses that cannot be economically recovered using normal crystallization methods, and is used as a raw material for the fermentation industry or as a compound feed. However, especially in Japan, the price of blackstrap molasses is extremely low compared to sugar, and sugar factories have traditionally tried to reduce the loss of sugar into the blackstrap molasses and improve the sugar recovery rate. Although efforts have been made to achieve this goal for many years, a method that is industrially and economically satisfactory has not yet been established.

Therefore, the present invention focused on membrane utilization technology, which has recently made remarkable progress, and conducted intensive studies on the application of a sugar solution purification method using a combination of ultrafiltration and electrodialysis, and as a result, has significantly improved the sugar recovery rate. This led to the invention of the new Hiko sugar production method.

However, there is no mention of a specific industrial method, and there is no mention of a specific method for recovering sugar by decocting and separating the purified sugar solution. In the cane raw material sugar production process, the sugar liquids to be purified are, in order of process, mixed juice, cleanliness, white syrup, and 1 to 1 to 100% molasses.

In order to clarify which part of the sugar manufacturing process the purification method of the present invention should be introduced into and what operating conditions should be used to obtain the most efficient purification method, the present inventors have investigated the ultrap-permeability , electrodialysis ability, decoction and separation properties, processing method of concentration chamber in ultrafiltration, etc., were comprehensively investigated and the results will be explained below.

First, Table 1 shows the results of a comparison of the membrane areas required for the ultra-P method and the electrodialysis method for various sugar solutions to be cleaned.

Table 1 (Examples 1 and 2, Comparative Examples 1 to 6) In the membrane cleaning method, the membrane equipment cost is extremely large in the cleaning cost. It is clear that molasses as a sugar material, ie, ■molasses in the case of the three-stage roasting sugar separation method, or final stage molasses, i.e. ■molasses, is economically advantageous. If the pre-process of the sugar brewing process, that is, the mixed juice, cleanliness, or syrup, is targeted for cleaning, not only the sugar recovery rate but also the quality of the sugar can be improved, but the cleaning equipment will be bulky and the equipment cost will increase. It has the disadvantage of being hugely publicized.

Moreover, in this case, there is no need to particularly improve the quality of the sugar raw material for cane by introducing a new purifying method.

Next, a decoction/separation test was conducted on the cleanliness, I molasses, and honey molasses treated by the cleaning method of the present invention. The results are shown in Table 2.

Table 2 compares the current sugar brewing method and the method of the present invention when the current sugar brewing method is set as 100, and the "time for brewing sugar and the amount of water added at the time of brewing sugar". (Example 3,
Comparative Example 7.8) Table 2 In Table 2, "water for pouring" refers to the water that is poured into the can to erase the parts that appear under the white part of the roasted sugar in the crystal can and leave only the normal crystals. means. From Table 2, compared to the current front-filling method,
When the same brewing sugar material is purified according to the present invention, the cleaning sugar time is only shortened to one value, but
It was revealed that for I molasses and U molasses, both the time for brewing sugar and the amount of water added were reduced to about 172 times compared to clean juice.

From the viewpoint of the cost of cleaning equipment, the most suitable sugar solutions to be purified by the present invention are molasses and molasses; On the other hand, in the case of molasses, the effect of energy saving, improvement of sugar quality and improvement of F1 sugar recovery rate is greatest for M and 11 white lower roasted sugars.

In other words, it has become clear that the effect is greatest when molasses is used as the object of purification.9.

Surprisingly, when molasses is the object of cleaning in the present invention, as shown in the following schematic diagram, 4.
The viscosity of white sugar is lower than that of the current five-stage roasted sugar separation method, and the viscosity of white sugar is lower than that of the current five-stage roasted sugar separation method, resulting in extremely good roasting properties. That's true.

The reason why these unexpected effects were obtained is thought to be that suspended solids, colloidal substances, and polymer substances were removed by ultrafiltration. It goes without saying that the linearity of the sugar solution increases as impurities are removed by ultrafiltration, but it also reduces the ability of the electrodialysis tank (q) in the next process due to blockages in the tank, membrane contamination, microbial contamination, etc. It also had a great effect on preventing accidents and stabilizing driving.

When summer molasses is the object of purification in the present invention, the purity of separated and recovered sugar, the recovery rate of sugar, and the linearity ratio of blackstrap molasses are compared with the current three-stage roasting and separation method, and the results are shown below.

Current method l Molasses 96j3 to 41 Linear axis ratio 55.2 to l Shishitaru-□□-----------□11 1 sugar 19.1 to 9 1 Molasses (blackstrap molasses) 73.6 k
g Pure bean ratio 96.5% Linear rate 66.6, this method M' Molasses 9-6.8 klJ Linear axis rate 53,29E From this result, compared with the current three-stage roasted sugar/separation method. In this method, the purity of sugar and the recovery rate of sugar were clearly increased, and the linearity ratio of blackstrap molasses was about 4 times lower. As a result of the increase in the recovery rate of sugar products, it has been revealed that the ratio of total sugar waste to JN materials will increase by at least 0.4%.

Next, a method for treating condensed honey in ultrapolar filtration will be explained. When molasses is subjected to ultrapolar treatment, a problem arises in which impurities are concentrated at the same time as the permeated molasses, that is, a concentration problem, but this concentration chamber is considered to be a waste liquid of one glaze, and the method of treatment is important.

The inventors of the present invention have also obtained new knowledge regarding an economical method for processing a concentration chamber through the series of tests already described. Concentration 1 has a high sugar content, so it is not suitable for wastewater treatment with microorganisms.
L. Additionally, the cost of evaporating, solidifying, and burning the water is enormous. Therefore, we sought operating conditions for ultrafiltration that would allow the sugar purity in the concentration chamber to be on the same level as the sugar purity of the blackstrap molasses used as a commercial product, and devised a treatment method in which the concentrate was directly mixed into the blackstrap molasses.

Here, sugar purity is the total sugar content divided by the Brix solid content and expressed as a percentage. Total sugar content means the sum of sucrose divided by 0°95 and total sugar content.

If the blackstrap molasses in the current S-stage roasting sugar separation method escapes from the ultra-F, the purity of the concentrate in the concentration chamber will drop below the sugar purity of the blackstrap molasses that is not subjected to ultrafiltration, and direct mixing will cause the blackstrap molasses to This is not desirable as it significantly reduces the product value. On the other hand, by ultrafiltrating the molasses and increasing the recovery rate of permeated solids in the molasses to 80-90% in terms of Brix solid content, the purity of sugar in the concentration chamber is 45-55, which is directly mixed into the molasses. However, it was found that the sugar purity of blackstrap molasses did not decrease and the commercial value could be maintained. The test results are as shown in Example 4.

The method of the present invention is not limited to the molasses used in the current three-stage roasted sugar method shown at the beginning, but can be applied to molasses, which is the final stage of roasted sugar, regardless of the method used. Good to have.

For example, even when purifying molasses using the four-stage roasting/separation method, the effects of the present invention, such as reduction in cleaning equipment costs, energy savings, and improvement in sugar recovery rate, remain the same, and the processing method in the concentration chamber remains unchanged. b0 Next, the present invention will be explained in more detail with reference to Examples and Comparative Examples, but it goes without saying that the present invention is not limited to these Examples.

Ultra-Pa test of various sugar solutions The equipment used was a heat-resistant back-type ultra-P filtration device manufactured by Daicel Chemical Industries, Ltd. (effective membrane surface 'yt was 2 to 8 = 2 m'/tube x 1 to 4 tubes). ).The membrane module is DMH-2
The effective membrane area #'i2- is 508 (a set type with 18 elements, per module). The material of the membrane is polyether sulfon, and the molecular weight cutoff is #'i40.00.
It is 0. ), and two of these modules were connected in series [2] and operated in batch mode.

The operating conditions were as follows: the clean juice had the same concentration, the molasses was diluted to a concentration of 40%, the temperature was 70°C, the inlet pressure of the connection module was 15kg/am'', and the flow rate LV = 1.9.
m/aeho, teh D, a over 7'! Ultrafiltration was performed until the solid content recovery rate was 85%.

The module was replaced with a new one for each case of sugar solution O, and a comparative test was conducted, and the results are shown in Table 5.

= 13 Example 2 and Comparative Examples 4, 5.6 The equipment used in the electrodialysis test for each AIO building was Asahi Glass (Kiku's DW-0 model 1d).
Air dialysis machine (effective membrane area is 2.54 m24 = 5.0
7 dm2/pair x 50 pairs), and the ion exchange membrane was a combination of OMV (cation membrane) and new MMV (fouling-resistant anion membrane), and was operated in a batch mode.

The operating conditions were the ultrafiltrated sugar solution t-stock solution of Example 1 and Comparative Examples 1 and 2.3, once at 35 °C, temperature at 55 °C, membrane surface flow rate LV-8110 cm/sec % transmembrane voltage 0.4
Electrodialysis was carried out at 5 V/pair to a desalination rate of 75.

The ion exchange membrane was replaced with a new one for each type of sugar solution and a comparative test was conducted, and the results are shown in Table 4.

1 Toku H evil 2-30000 (7) sides! Example 5 and Comparative Example 7.8 Separation test of each syrup solution The apparatus used was a Chubu-made shaft (a calandria type designed and manufactured by Rinko). This is a Kusaka Charge 2-liter centrifugal separator with a basket diameter of 9 inches, a number of rotations of 400 ORPM, and a 60-liter crystal can and mud controller, a 60-liter crystallizer, and a domestically produced centrifuge.

The test sugar solutions are the sugar solutions of Example 2 and Comparative Examples 4 and 5 that have been subjected to ultrafiltration and electrodialysis.

The operating methods for roasting sugar, auxiliary crystals, and separation were similar to those currently used in ordinary factories, and in particular, roasting sugar was carried out by one skilled sugar roaster.

The results are shown in Table 5.

In particular, in the case of the present invention, the purity of the separated and recovered sugar was higher than that by the current method, and the sugar recovery rate was greater than the value calculated from the rise of the sugar solution on the wire shaft. The linearity of the 'W molasses (blackstrap molasses) obtained by the final stage of roasting and separation according to the present invention is about 4 lower than that of the current I molasses (blackstrap molasses).

Example 4 Ultrafiltration test of molasses as the final stage roasted sugar material Under the operating conditions similar to Example 1, ultrafiltration test of molasses (nm molasses) as the final stage roasted sugar material targeted by the present invention was conducted. FIG. 1 shows the results of a test regarding the relationship between "Permeation Brix Solid Content Recovery Rate" and "Sugar Purity of Concentrated Honey."

[Brief explanation of drawings]

FIG. 1 shows the changes over time in the "permeation Brix solid envelope yield" and the "sugar purity of dark condensed honey" in molasses, which is the final stage roasted sugar material according to the method of the present invention. Engraving of the drawings (no changes to the contents) Figure 1 Ultra-penetration time (hrsl- procedure?ili IF document (method) % formula % 1. Indication of the incident 1985 Patent Application No. 167646 2. Title of the invention [1 ↑Recovery method for raw sugar from raw cane” 3. Relationship with the case of the person making the amendment Applicant name: Mitsui Sugar Co., Ltd. 4. Agent (3 persons) Address: ◎
105 8-1 Toranomon 2-chome, Minato-ku, Tokyo (Toranomon Denki Building) Applicant's furigana tlii (application for correction), head number column on the left side of the application. (Contents: 2 No changes) 6. Contents of the amendment Procedure as per attached sheet ↑ Correct ■: October 24, 1985 Director General of the Patent Office Michi Uga Department 1, Indication of the case Patent Application No. 167646 of 1985 No. 2, Name of the invention [↑Recovery method for raw sugar from raw potato 33 Relationship with the case of the person making the amendment Applicant name: Mitsui Sugar Co., Ltd. (and 3 others) 4. Agent address: [Co., Ltd.] 105 Toranomon, Minato-ku, Tokyo 2-8-1 (
Toranomon Electric Building) [Telephone: 03 (502) 1476 (Representative)] 5 Subject of amendment Name of the invention of Meiwa 1st Petty Officer Detailed description of the invention in the specification Column Drawings & Contents of amendment 1, Name of the invention is corrected as below. "Method for recovering sugar raw material for cane" 2) At the end of page 6 of the specification, "the present invention, etc." is corrected to "the present inventors, etc." 3) "Electrodialysis method" in the 5th line from the bottom of the 1st page, the 1st and 5th lines of the 4th page, the 1st line of the 5th page, and in Cloth 1, changed to "electrodialysis method", the bottom of the 4th page. From line 4, “Electro-dialysis 4JT ability” to “electrodialysis ability,” page 15, line 2, “electrodialysis test” to “electrodialysis test,” page 15, line 4 and 16 Sadasue line, “electrodialysis ability.” "dialysis machine" changed to "electrodialysis machine" on page 15, page 4
Correct the line ``electrodialysis'' to ``electrodialysis,'' and correct the line 5 from the bottom of page 16, page 17, ``electrodialysis treatment,'' to ``electrodialysis treatment.'' 4) Correct the 6th line of No. 10, "Sugar supplementation rate 57.0%" to "Sugar supplementation rate 67.0%." 5) Page 14, Table 5, Number 6, “Insanity/Brix solid content”
1 sugar content/Brix solids", column 5 of the same table "(ton/1'000 tons of cane)"
15)
The first line of the page, "Example 2 and Comparative Example 4.5.6", has been corrected to "Example and Comparative Example 4.5.6". 7) Change the 3rd column of the 4th coat, "Ash content of Brix solid fraction" to "(C) Ash content % of the Brix solid fraction" on page 16, and change the 5th column of the 4th coat, "(tons/1 ton of cane)" )” as well as Section 6 of the same table.
Make corrections in the column. 8) Change “Example 6 and Comparative Example 7.8” to “Example 6 and Comparative Example 7.8” on page 17, line 1.
Corrected to "Example 3 and Comparative Examples 7.8". 9) Add "(hours-minutes)" next to the sixth column of Table 5 on page 18, "Pre-sugar time". 10) Correct the drawing as shown in the attached sheet. Figure 1 Limit 1 suitable time (hrs) -

Claims (1)

[Scope of Claims] 1. When recovering sugar by cleaning the sugar solution in the cane raw material sugar manufacturing process by ultrafiltration and electrodialysis, it is recognized that the sugar solution is molasses that will be the final stage of decocted sugar material. Characteristic sugar recovery method. 2. The sugar recovery method according to claim 1, wherein the solid content recovery rate of permeated molasses in the ultrafiltration method is in the range of 80 to 90% in terms of Brix solid content.