CN110819741A - Method for removing pigment in syrup by using rosin-based anion macroporous adsorption resin - Google Patents
Method for removing pigment in syrup by using rosin-based anion macroporous adsorption resin Download PDFInfo
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- CN110819741A CN110819741A CN201911037553.3A CN201911037553A CN110819741A CN 110819741 A CN110819741 A CN 110819741A CN 201911037553 A CN201911037553 A CN 201911037553A CN 110819741 A CN110819741 A CN 110819741A
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- rosin
- syrup
- adsorption resin
- macroporous adsorption
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- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B20/00—Purification of sugar juices
- C13B20/12—Purification of sugar juices using adsorption agents, e.g. active carbon
- C13B20/126—Organic agents, e.g. polyelectrolytes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28085—Pore diameter being more than 50 nm, i.e. macropores
Abstract
The invention discloses a method for removing pigment in syrup by using rosin-based anionic macroporous adsorption resin, belonging to the technical field of syrup refining. The invention adds rosin-based anion macroporous adsorption resin into syrup, adopts a static adsorption method, and controls the dosage of the rosin-based anion macroporous adsorption resin to be 0.01-0.5 g.mL‑1The temperature is 30-80 ℃, the adsorption time is 0.5-24h, the pigment in the syrup is well removed, and the removal rate of the pigment in the syrup can reach more than 90%. The rosin-based anion macroporous adsorption resin after saturated adsorption is washed and regenerated, and the resin can be reused, is safe, environment-friendly, non-toxic, low in cost and suitable for popularization and application.
Description
Technical Field
The invention belongs to the technical field of syrup refining, and particularly relates to a method for removing pigment in syrup by using rosin-based anionic macroporous adsorption resin.
Background
In the production of sucrose, the color value of sugar is an important indicator. When the sugar juice is evaporated and concentrated at high temperature, reducing sugar and amino acid can continuously generate Maillard reaction to produce melanoidin pigment, so that the color value of the sugar juice is increased. The melanoidins produced remain in the crystals during sucrose crystallization, resulting in a higher color value of granulated sugar. Therefore, there is a need to remove melanoidin pigment from syrup.
The methods commonly used in the sugar industry to remove melanoidin pigment at present mainly include:
1. heiguan, Liangxianhui, etc., the influence of clarification process conditions of a sulfurous method cane sugar factory on the phenol removal and decoloration effects of cane juice [ J ] food industry 2015, 112-115, wherein the sulfurous method is used for cane juice clarification.
2. Living, ceramic membrane filtration behavior mechanism and key problem study of sugarcane mixed juice clarification [ D ] university of cantonese, 2018: 116, 141, wherein use of ceramic membranes to remove pigments from syrups is mentioned.
3. Chinese patent 102020745B discloses a novel acrylic acid series decolorizing resin and a preparation method thereof, vinyl pyridine monomer and aliphatic unsaturated ester monomer are adopted, polyvinyl monomer is taken as cross-linking agent, suspension polymerization is carried out in the presence of pore-forming agent to obtain white spheres, the obtained white spheres and polyethylene polyamine are subjected to aminolysis reaction to introduce amido, the obtained amine spheres and monomer containing alcoholic hydroxyl are reacted under alkaline condition to obtain the acrylic acid series ion exchange decolorizing resin, and the resin has the properties of strong base resin containing pyridine group and weak base resin. However, the raw materials are mainly pyridine compounds, have certain carcinogenicity and potential food safety hazards, and are difficult to separate in food grade.
Luo J, Hang X, et al, refining sugar juice by an integrated Membrane process, Filtration behavor of polymeric Membrane at high brightness and [ J ] Journal of Membrane Science,2016,509:105 and 115, wherein the use of polymeric membranes to remove pigments from sugarcane juice is mentioned.
Although the membrane technology can retain nearly 100% of suspended impurities and most of pigments in the cane juice, the retention rate of the membrane technology to reducing sugar and amino acid in the cane juice is low, so that the reducing sugar and the amino acid continuously undergo Maillard reaction in the subsequent process of the cane juice, the color value of the cane juice is increased again, and in addition, the problems of membrane pollution, high production cost and the like are difficult to solve, so that the membrane technology is rarely used. Therefore, the macroporous adsorption resin method is gradually paid attention to in the sugar industry, and the macroporous adsorption resin method utilizes exchange groups and abundant pore structures of the resin for adsorption and exchange. However, at present, no adsorption resin which is safe and environment-friendly and has an obvious effect of removing pigments in syrup exists, so that an adsorption resin which is safer and environment-friendly and has better adsorption performance is needed to be found for removing the pigments in the syrup.
Disclosure of Invention
Aiming at the problems, the invention provides a method for removing pigment in syrup by using rosin-based anionic macroporous adsorption resin, which is safe and environment-friendly and has obvious effect of removing pigment in syrup.
The invention is realized by the following technical scheme:
a method for removing pigment from syrup by using rosin-based anionic macroporous adsorption resin comprises the steps of adding the rosin-based anionic macroporous adsorption resin into the syrup, and adopting a static adsorption method, wherein the dosage of the rosin-based anionic macroporous adsorption resin is controlled to be 0.01-0.5 g/mL-1The temperature is 30-80 ℃, and the adsorption time is 0.5-24 h; the structural formula of the rosin-based anion macroporous adsorption resin is as follows:
wherein R is:
the static adsorption method is a method in which a certain amount of adsorbent and a certain amount of solution are brought into sufficient contact for a long time to reach equilibrium; the static adsorption method is a method for balancing a certain amount of rosin-based anion macroporous adsorption resin and a certain amount of syrup by fully contacting for a long time.
Preferably, the method adopts a static adsorption method by adding the rosin-based anion macroporous adsorption resin into the syrup, and the dosage of the rosin-based anion macroporous adsorption resin is controlled to be 0.1-0.3 g/mL-1The temperature is 50-70 ℃, and the adsorption time is 5-10 h.
Preferably, the method adopts a static adsorption method by adding the rosin-based anion macroporous adsorption resin into the syrup, and the dosage of the rosin-based anion macroporous adsorption resin is controlled to be 0.2 g/mL-1The temperature is 60 ℃, and the adsorption time is 6 h.
Preferably, the rosin-based anion macroporous adsorption resin is a spherical porous material, the average pore diameter of the rosin-based anion macroporous adsorption resin is 10-35nm, and the specific surface area of the rosin-based anion macroporous adsorption resin is 10-20m2/g。
The rosin-based anion macroporous adsorption resin is prepared by adopting the patent technology 'rosin-based anion macroporous adsorption resin and a preparation method thereof' which is applied by the applicant on the same day.
The rosin-based anion macroporous adsorption resin has a removal rate of more than 80% to pigment in syrup.
The rosin-based anion macroporous adsorption resin can be repeatedly used, and comprises the following steps: washing the rosin-based anionic macroporous adsorption resin which is adsorbed and saturated in the syrup by using water to remove residual syrup and impurities, then converting the resin into an anionic type by using a 2% NaOH solution, and washing the rosin-based anionic macroporous adsorption resin by using water until the rosin-based anionic macroporous adsorption resin is close to neutral.
The adsorption and regeneration principle of the rosin-based anion macroporous adsorption resin is as follows:
(1) the adsorption process of the resin is as follows:
R(OH-)+R1 -→R2R1 -+OH-；
(2) the regeneration process of the resin comprises the following steps: r2R1 -+OH-→R(OH-)+R1 -(ii) a Wherein R is1 -Representing negatively charged pigment molecules.
The resin adsorption process mainly comprises the following steps: functional group-N on resin+(CH3)3OH-With pigment molecules R1 -Ion exchange takes place. After the resin is adsorbed and saturated, the resin is converted into anion by using 0.01-5% NaOH solution, and can be recycled.
Compared with the prior art, the invention has the advantages and beneficial effects that:
(1) the rosin-based anion macroporous adsorption resin is a polyester polymer material synthesized by taking rosin as a raw material, has the performance of complete biodegradation, is green and environment-friendly in the process of removing pigments in syrup, has the characteristic of no toxicity, and is suitable for being used in syrup; and the mechanical strength is high, the pressure resistance is strong, the cost is low, and the application prospect is good.
(2) The rosin-based anion macroporous adsorption resin applied by the invention has a good removal effect on pigments in syrup, and the removal rate of the pigments in the syrup is more than 80%. The rosin-based anion macroporous adsorption resin after saturated adsorption can be reused after being washed and regenerated, the adsorption capacity of the rosin-based anion macroporous adsorption resin on pigment in syrup can still reach more than 56% after 10 times of repeated use, and the application prospect is good.
(3) When the adding amount of the rosin-based anion macroporous adsorption resin is controlled to be 0.1-0.3 g/mL-1The temperature is 50-70 ℃, the adsorption time is 5-10h, the removal effect on the pigment in the syrup is good, and the removal rate can reach more than 90%; particularly when the adding amount of the rosin-based anion macroporous adsorption resin is controlled to be 0.2 g/mL-1The temperature is 60 ℃, the adsorption time is 6h, and the adsorption time is 6h for syrupThe pigment removal effect is best, and the removal rate can reach 92.25%.
Drawings
FIG. 1 is a graph showing the result of the reusability of rosin-based anionic macroporous adsorbent resin for removing pigments from syrup in example 9 of the present invention;
FIG. 2 is a graph showing the effect of the rosin-based anionic macroporous adsorbent resin on the dynamic adsorption performance of syrup for removing pigments in the syrup according to example 10 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following description of specific embodiments and accompanying drawings, but the present invention is not limited thereto.
The structural formula of the rosin-based anion macroporous adsorption resin used in the invention is as follows:
wherein R is:
the average pore diameter of the rosin-based anion macroporous adsorption resin is 10-35nm, and the specific surface area is 10-20m2(ii) in terms of/g. The rosin-based terpolymer is prepared by a patent technology of a rosin-based terpolymer and a preparation method thereof which is disclosed by the applicant on the same day.
Example 1
10g of rosin-based anion macroporous adsorption resin is added into 50mL of syrup, and the mixture is shaken at constant temperature of 60 ℃ for 6 hours. The removal rate of the pigment was 92.25%.
Example 2
15g of rosin-based anion macroporous adsorption resin is added into 50mL of syrup, and the mixture is shaken at constant temperature of 70 ℃ for 10 hours. The removal rate of the pigment was 90.12%.
Example 3
7.5g of rosin-based anion macroporous adsorbent resin is added into 50mL of syrup, and the mixture is shaken at constant temperature of 55 ℃ for 8 hours. The removal rate of the pigment was 87.12%.
Example 4
5g of rosin-based anion macroporous adsorption resin is added into 50mL of syrup, and the mixture is shaken at constant temperature of 50 ℃ for 5 hours. The removal rate of the pigment was 86.75%.
Example 5
2.5g of rosin-based anion macroporous adsorption resin is added into 50mL of syrup, and the mixture is shaken at constant temperature of 65 ℃ for 15 h. The removal rate of the pigment was 86.33%.
Example 6
20g of rosin-based anion macroporous adsorption resin is added into 50mL of syrup, and the mixture is shaken at constant temperature of 40 ℃ for 3 hours. The removal rate of the pigment was 86.56%.
Example 7
0.5g of rosin-based anion macroporous adsorption resin is added into 50mL of syrup, and the mixture is shaken at constant temperature of 30 ℃ for 24 hours. The removal rate of the pigment was 85.56%.
Example 8
25g of rosin-based anion macroporous adsorption resin is added into 50mL of syrup, and the mixture is shaken at constant temperature of 80 ℃ for 0.5 h. The removal rate of the pigment was 82.25%.
Example 9
The rosin-based anionic macroporous adsorbent resin saturated in the syrup in example 1 was washed with water to remove residual syrup and impurities, the resin was then converted to anionic form with 2% NaOH solution, and the rosin-based anionic macroporous adsorbent resin was washed with water until it was nearly neutral.
The results of 10 times of repeated use of the rosin-based anionic macroporous adsorbent resin are shown in FIG. 1, and it can be seen from FIG. 1 that the removal rate of the pigment in the syrup when the rosin-based anionic macroporous adsorbent resin is used for the first time is 1.1mg g-1The removal rate of the pigment in the syrup can still reach nearly 0.8 mg/g after the syrup is repeatedly used for 10 times-1More than 70 percent of the rosin-based anion macroporous adsorption resin is used for the first time, so that the rosin-based anion macroporous adsorption resin has good reusability.
The same reusability test was performed on the rosin-based anionic macroporous adsorbent resins of examples 2 to 8 after saturation in syrup, and the obtained test results are highly consistent, indicating that the rosin-based anionic macroporous adsorbent resins have good reusability.
Example 10
In a column with an internal diameter of 1.5cm and a height of 20cmThe adsorption column is filled with rosin-based anion macroporous adsorption resin, the adsorption column is vibrated continuously in the filling process to ensure uniform distribution, the rosin-based anion macroporous adsorption resin in the column is soaked in pure water for 12 hours before an experiment, and absorbent cotton is added at the top to ensure uniform liquid distribution; then, 3g of resin was packed in the column, the temperature was controlled at 60 ℃ and the flow rate was controlled at 2 mL/min-1(ii) a The effluent was collected and its dynamic adsorption curve was measured, and the results are shown in FIG. 2. As can be seen from FIG. 2, the removal amount of Maillard pigment by the rosin-based anion macroporous adsorption resin can reach 1.02 mg.g-1Therefore, the rosin-based anion macroporous adsorption resin has a good effect of removing pigments in syrup.
Claims (5)
1. A method for removing pigment in syrup by using rosin-based anionic macroporous adsorption resin is characterized in that the method is to add the rosin-based anionic macroporous adsorption resin into the syrup and adopt a static adsorption method, and the dosage of the rosin-based anionic macroporous adsorption resin is controlled to be 0.01-0.5 g.mL-1The temperature is 30-80 ℃, and the adsorption time is 0.5-24 h; the structural formula of the rosin-based anion macroporous adsorption resin is as follows:
wherein R is:
2. the method for removing pigment in syrup by using the rosinyl anion macroporous adsorption resin as claimed in claim 1, wherein the method is to add the rosinyl anion macroporous adsorption resin into the syrup by a static adsorption method, and the dosage of the rosinyl anion macroporous adsorption resin is controlled to be 0.1-0.3 g-mL-1The temperature is 50-70 ℃, and the adsorption time is 5-10 h.
3. Use of rosin-based anions according to claim 2The method for removing pigment in syrup by using macroporous adsorption resin is characterized in that the method is that rosin-based anion macroporous adsorption resin is added into syrup, a static adsorption method is adopted, and the dosage of the rosin-based anion macroporous adsorption resin is controlled to be 0.2 g/mL-1The temperature is 60 ℃, and the adsorption time is 6 h.
4. The method for removing pigment in syrup by using the rosin-based anionic macroporous adsorption resin as claimed in any one of claims 1 to 3, wherein the rosin-based anionic macroporous adsorption resin is a spherical porous material with an average pore diameter of 10 to 35nm and a specific surface area of 10 to 20m2/g。
5. The method for removing pigment in syrup by using the rosin-based anionic macroporous adsorption resin as claimed in any one of claims 1 to 3, wherein the removal rate of the rosin-based anionic macroporous adsorption resin on the pigment in the syrup is 80% or more.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112408547A (en) * | 2020-10-16 | 2021-02-26 | 广西民族大学 | Water softening method |
Citations (4)
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|---|---|---|---|---|
| JPH02265926A (en) * | 1989-04-07 | 1990-10-30 | Kao Corp | New siloxane derivative, and cosmetic lubricant and cosmetic containing same |
| CN101768240A (en) * | 2010-01-26 | 2010-07-07 | 广西民族大学 | Abietyl-containing terpolymer and preparation method thereof |
| CN107529536A (en) * | 2017-08-18 | 2018-01-02 | 广西民族大学 | A kind of low pole rosinyl polymer microsphere and its preparation method and application |
| CN109999763A (en) * | 2019-03-20 | 2019-07-12 | 广西民族大学 | A kind of method of calcium ions and magnesium ions in removal syrup |
-
2019
- 2019-10-29 CN CN201911037553.3A patent/CN110819741B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02265926A (en) * | 1989-04-07 | 1990-10-30 | Kao Corp | New siloxane derivative, and cosmetic lubricant and cosmetic containing same |
| CN101768240A (en) * | 2010-01-26 | 2010-07-07 | 广西民族大学 | Abietyl-containing terpolymer and preparation method thereof |
| CN107529536A (en) * | 2017-08-18 | 2018-01-02 | 广西民族大学 | A kind of low pole rosinyl polymer microsphere and its preparation method and application |
| CN109999763A (en) * | 2019-03-20 | 2019-07-12 | 广西民族大学 | A kind of method of calcium ions and magnesium ions in removal syrup |
Non-Patent Citations (2)
| Title |
|---|
| 张冬民: "含葡萄糖基松香基大孔吸附树脂的合成及吸附性能的研究", 《中国优秀硕士学位论文全文数据库》 * |
| 赵勇等: "马来松香丙烯酸甘油酯大孔吸附树脂对芸香叶苷的吸附性能研究", 《广西民族大学学报(自然科学版)》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112408547A (en) * | 2020-10-16 | 2021-02-26 | 广西民族大学 | Water softening method |
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