Purification method of populus diversifolia alkali

Abstract

The invention provides a purification method of populus diversifolia alkali, and belongs to the technical field of purification and impurity removal. According to the method, the activated carbon is sequentially subjected to alkali treatment and acid treatment to obtain the activated carbon, then the activated carbon is adopted to perform decoloration treatment on the populus diversifolia alkali stock solution, impurities in the populus diversifolia alkali stock solution are removed, and the decoloration rate is increased. Results of the embodiment show that after the purification method is adopted, the decolorization rate of the populus diversifolia alkali stock solution can reach about 83%.

Description

Technical Field

[0001] The present invention belongs to the technical field of purification and impurity removal, and particularly relates to a method for purifying poplar alkali. Background Art

[0002] Poplar alkali is the secretion of poplar tree branches and trunks, also known as poplar tears and poplar tree tears. It can be used to treat gastric distension, sore throat, duodenal ulcer, etc., and can also be used for making naan and steaming steamed buns.

[0003] Currently, poplar alkali is mainly directly used after being washed or extracted with a solvent, but it still contains some impurities, which limits its application in some fields.

[0004] Therefore, there is an urgent need for a method for purifying poplar alkali. Summary of the Invention

[0005] The purpose of the present invention is to provide a method for purifying poplar alkali. After being treated with the purification method of the present invention, the poplar alkali stock solution has excellent decolorization effect.

[0006] In order to achieve the above-mentioned invention purpose, the present invention provides the following technical solutions:

[0007] The present invention provides a method for purifying poplar alkali, comprising the following steps:

[0008] (1) Mix poplar alkali with water and perform ultrasonic extraction to obtain a poplar alkali stock solution;

[0009] (2) Mix activated carbon with an alkali solution and perform alkali treatment to obtain alkali-treated activated carbon;

[0010] (3) Mix the alkali-treated activated carbon obtained in step (2) with an acid solution and perform acid treatment to obtain activated activated carbon;

[0011] (4) Mix the poplar alkali stock solution obtained in step (1) and the activated activated carbon obtained in step (3) and perform decolorization treatment to obtain a poplar alkali extract;

[0012] There is no sequence requirement between step (1) and steps (2) to (3).

[0013] Preferably, the particle size of the poplar alkali in step (1) is ≤60 mesh.

[0014] Preferably, the mass ratio of poplar alkali to the volume of water in step (1) is 1 g:(35 - 45) mL.

[0015] Preferably, the temperature of ultrasonic extraction in step (1) is 45 - 55 °C, the time of ultrasonic extraction is 10 - 20 min, and the power of ultrasonic extraction is 420 - 540 W.

[0016] Preferably, the mass concentration of the alkali solution in step (2) is 3-7%.

[0017] Preferably, the time of alkali treatment in step (2) is 20-30 min.

[0018] Preferably, the concentration of the acid solution in step (3) is 4-8 mol / L.

[0019] Preferably, the time of acid treatment in step (3) is 20-30 min.

[0020] Preferably, the mass ratio of the activated carbon to the original solution of poplar alkali in step (4) is (5-5.5) g: 100 mL.

[0021] Preferably, the temperature of the decolorization treatment in step (4) is 50-55 °C, the time of the decolorization treatment is 80-85 min, and the pH value of the decolorization treatment is 8-9.

[0022] The present invention provides a method for purifying poplar alkali, comprising the following steps: (1) mixing poplar alkali with water and performing ultrasonic extraction to obtain the original solution of poplar alkali; (2) mixing activated carbon with an alkali solution and performing alkali treatment to obtain alkali-treated activated carbon; (3) mixing the alkali-treated activated carbon obtained in step (2) with an acid solution and performing acid treatment to obtain activated carbon; (4) mixing the original solution of poplar alkali obtained in step (1) and the activated carbon obtained in step (3) and performing decolorization treatment to obtain the poplar alkali extract; there is no sequence between step (1) and steps (2)-(3). The present invention sequentially performs alkali treatment and acid treatment on activated carbon to obtain activated carbon, and then uses the activated carbon to perform decolorization treatment on the original solution of poplar alkali to remove impurities in the original solution of poplar alkali and improve the decolorization rate. The results of the examples show that after using the purification method of the present invention, the decolorization rate of the original solution of poplar alkali can reach about 83%. Description of the Drawings

[0023] Figure 1 It is a macroscopic view of the poplar alkali extract obtained in step (3) of Example 1;

[0024] Figure 2 It is a macroscopic view of the poplar alkali extracts obtained in Comparative Examples 1-5. Detailed Embodiments

[0025] The present invention provides a method for purifying poplar alkali, comprising the following steps:

[0026] (1) Mixing poplar alkali with water and performing ultrasonic extraction to obtain the original solution of poplar alkali;

[0027] (2) Mixing activated carbon with an alkali solution and performing alkali treatment to obtain alkali-treated activated carbon;

[0028] (3) Mix the alkali-treated activated carbon obtained in step (2) with an acid solution for acid treatment to obtain activated activated carbon;

[0029] (4) Mix the populin original solution obtained in step (1) with the activated activated carbon obtained in step (3) for decolorization treatment to obtain a populin extract;

[0030] There is no order of priority between step (1) and steps (2)-(3).

[0031] Unless otherwise specified, the present invention does not have special limitations on the sources of various raw materials, and commercially available products well-known to those skilled in the art can be used.

[0032] In the present invention, populin is mixed with water and subjected to ultrasonic extraction to obtain a populin original solution.

[0033] The present invention does not have special limitations on the source of the populin, and populin from well-known sources to those skilled in the art can be used.

[0034] In the present invention, the particle size of the populin is preferably ≤60 mesh.

[0035] In the present invention, when the particle size of the populin is not within the above range, the present invention preferably pulverizes the populin and then sieves it.

[0036] The present invention does not have special limitations on the operations of pulverization and sieving, and technical solutions well-known to those skilled in the art can be used to ensure that the particle size of the populin after pulverization and sieving is within the above range.

[0037] In the present invention, the water is preferably ultrapure water.

[0038] In the present invention, the mass ratio of the populin to the volume of water is preferably 1 g:(35-45) mL. As an implementation manner, the mass ratio of the populin to the volume of water can specifically be 1 g:35 mL, 1 g:37 mL, 1 g:39 mL, 1 g:40 mL, 1 g:41 mL, 1 g:43 mL, or 1 g:45 mL.

[0039] In the present invention, the temperature of the ultrasonic extraction is preferably 45-55 °C. As an implementation manner, the temperature of the ultrasonic extraction can specifically be 45 °C, 48 °C, 50 °C, 52 °C, or 55 °C.

[0040] In the present invention, the time of the ultrasonic extraction is preferably 10-20 min. As an implementation manner, the time of the ultrasonic extraction can specifically be 10 min, 12 min, 15 min, 18 min, or 20 min.

[0041] In the present invention, the power of the ultrasonic extraction is preferably 420 - 540 W. As an embodiment, the power of the ultrasonic extraction may specifically be 420 W, 450 W, 480 W, 500 W or 540 W. By controlling the dosages of the respective raw materials, the temperature, time and power of the ultrasonic extraction within the above ranges, the extraction rate of populin can be further increased in the present invention.

[0042] After the ultrasonic extraction is completed, the present invention preferably centrifuges and filters the product after the ultrasonic extraction in sequence to obtain the crude populin solution.

[0043] In the present invention, the speed of the centrifugation is preferably 4000 - 6000 r / min, more preferably 5000 r / min; the time of the centrifugation is preferably 5 - 15 min, more preferably 10 min.

[0044] In the present invention, the filtration is preferably vacuum filtration. The present invention has no special limitation on the operation of the vacuum filtration, and the solid impurities after centrifugation can be removed by adopting the technical solution of vacuum filtration well-known to those skilled in the art to obtain the filtrate.

[0045] After the filtration is completed, the present invention preferably dries and weighs the filter residue obtained by the filtration.

[0046] In the present invention, the temperature of the drying is preferably 110 - 130 °C, more preferably 120 °C; the time of the drying is preferably 2 - 4 h, more preferably 3 h.

[0047] In the present invention, the extraction rate of populin is preferably calculated according to the following formula I:

[0048] Extraction rate of populin % = (M - a) / M × 100% Formula I;

[0049] In the formula I, M is the mass of populin, and a is the mass of the filter residue after filtration and drying.

[0050] The present invention mixes activated carbon and an alkali solution and performs alkali treatment to obtain alkali-treated activated carbon.

[0051] In the present invention, the activated carbon is preferably phosphorus-free activated carbon. As an embodiment, the phosphorus-free activated carbon is purchased from Beijing Solarbio Science & Technology Co., Ltd., analytical pure.

[0052] In the present invention, the alkali solution is preferably an aqueous sodium hydroxide solution; the mass concentration of the alkali solution is preferably 3 - 7%, more preferably 4 - 6%, and further preferably 5%.

[0053] The present invention has no special limitation on the dosage of the alkali solution, and it is sufficient to submerge the activated carbon.

[0054] In the present invention, the alkali treatment is preferably carried out under boiling conditions; the time of the alkali treatment is preferably 20 to 30 minutes. By controlling the parameters of the alkali treatment within the above ranges, the present invention can further improve the decolorization effect of the activated carbon.

[0055] After the alkali treatment is completed, the present invention preferably filters and washes the product of the alkali treatment in sequence to obtain alkali-treated activated carbon.

[0056] The present invention has no special limitation on the operation of the filtration, and a solid can be obtained by adopting the filtration technical solution well-known to those skilled in the art.

[0057] The present invention has no special limitation on the operation of the water washing, and it can be washed to neutral by adopting the technical solution well-known to those skilled in the art.

[0058] After obtaining the alkali-treated activated carbon, the present invention mixes the alkali-treated activated carbon with an acid solution for acid treatment to obtain activated activated carbon.

[0059] In the present invention, the acid solution is preferably hydrochloric acid; the concentration of the acid solution is preferably 4 to 8 mol / L, more preferably 5 to 7 mol / L, and further preferably 6 mol / L.

[0060] The present invention has no special limitation on the dosage of the acid solution, and it is only necessary to submerge the alkali-treated activated carbon.

[0061] In the present invention, the acid treatment is preferably carried out under boiling conditions; the time of the acid treatment is preferably 20 to 30 minutes. By controlling the parameters of the acid treatment within the above ranges, the present invention can further improve the decolorization effect of the activated carbon.

[0062] After the acid treatment is completed, the present invention preferably filters, washes and dries the product of the acid treatment in sequence to obtain activated activated carbon.

[0063] The present invention has no special limitation on the operation of the filtration, and a solid can be obtained by adopting the filtration technical solution well-known to those skilled in the art.

[0064] The present invention has no special limitation on the operation of the water washing, and it can be washed to neutral by adopting the technical solution well-known to those skilled in the art.

[0065] In the present invention, the temperature of the drying is preferably 110 to 130 °C, more preferably 120 °C. The present invention has no special limitation on the time of the drying, and it can be dried to constant weight.

[0066] After obtaining the poplar alkali stock solution and the activated activated carbon, the present invention mixes the poplar alkali stock solution and the activated activated carbon for decolorization treatment to obtain a poplar alkali extract.

[0067] In the present invention, the mass-volume ratio of the activated carbon to the original solution of poplar alkali is preferably (5 - 5.5) g : 100 mL. As an embodiment, the mass-volume ratio of the activated carbon to the original solution of poplar alkali can specifically be 5 g : 100 mL, 5.1 g : 100 mL, 5.2 g : 100 mL, 5.3 g : 100 mL, 5.4 g : 100 mL, or 5.5 g : 100 mL.

[0068] In the present invention, the temperature of the decolorization treatment is preferably 50 - 55 °C. As an embodiment, the temperature of the decolorization treatment can specifically be 50 °C, 51 °C, 52 °C, 53 °C, 54 °C, or 55 °C.

[0069] In the present invention, the time of the decolorization treatment is preferably 80 - 85 min. As an embodiment, the time of the decolorization treatment can specifically be 80 min, 81 min, 82 min, 83 min, 84 min, or 85 min.

[0070] In the present invention, the pH value of the decolorization treatment is preferably 8 - 9. As an embodiment, the pH value of the decolorization treatment can specifically be 8, 8.5, or 9. The present invention preferably adds an acid to adjust the pH value of the decolorization treatment. In the present invention, the acid is preferably citric acid. The present invention uses citric acid to adjust the pH value. Citric acid is an edible weak acid, which enables the poplar alkali extract to be used in the food field. By controlling the dosages of the raw materials, the temperature, time, and pH value of the decolorization treatment within the above ranges, the decolorization effect can be further improved.

[0071] After the decolorization treatment is completed, the present invention preferably centrifuges and filters the product of the decolorization treatment in sequence to obtain the poplar alkali extract.

[0072] In the present invention, the speed of the centrifugation is preferably 4000 - 6000 r / min, more preferably 5000 r / min; the time of the centrifugation is preferably 5 - 15 min, more preferably 10 min.

[0073] In the present invention, the filtration is preferably vacuum filtration. The present invention has no special limitation on the operation of the vacuum filtration. The solid impurities can be removed by adopting the technical solution of vacuum filtration well-known to those skilled in the art to obtain the filtrate.

[0074] The present invention sequentially performs alkali treatment and acid treatment on activated carbon to obtain activated carbon, and then uses the activated carbon to perform decolorization treatment on the original solution of poplar alkali, removes the impurities in the original solution of poplar alkali, controls the parameters in the purification process, and improves the decolorization rate.

[0075] The technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without making creative efforts fall within the scope of protection of the present invention.

[0076] Example 1

[0077] A method for purifying poplar alkali: (1) Grind poplar alkali into powder with a pulverizer, pass through a 60-mesh sieve to obtain poplar alkali powder. Mix the poplar alkali powder with ultrapure water and perform ultrasonic extraction. The mass ratio of poplar alkali powder to the volume of ultrapure water is 1 g:40 mL. The temperature of ultrasonic extraction is 50 °C, the time of ultrasonic extraction is 15 min, and the power of ultrasonic extraction is 480 W. After ultrasonic extraction is completed, centrifuge at 5000 r / min for 10 min and perform vacuum filtration to obtain the original poplar alkali solution;

[0078] (2) Soak phosphorus-free activated carbon (Beijing Solarbio Science & Technology Co., Ltd., analytical pure) in a sodium hydroxide aqueous solution with a mass concentration of 5%, boil for 30 min and then filter. Rinse with deionized water until neutral, then soak in 6 mol / L hydrochloric acid, boil for 30 min and then filter. Rinse with deionized water until neutral and dry at 120 °C to obtain activated carbon;

[0079] (3) Mix the activated carbon and the original poplar alkali solution and perform decolorization treatment. The mass ratio of activated carbon to the volume of the original poplar alkali solution is 5.3 g:100 mL. The temperature of decolorization treatment is 51 °C, the time of decolorization treatment is 82 min, and the pH value of decolorization treatment is 8.5. After decolorization treatment is completed, centrifuge at 5000 r / min for 10 min and perform vacuum filtration to obtain the poplar alkali extract.

[0080] Test the decolorization rate of the poplar alkali extract in step (3) of Example 1 three times.

[0081] The decolorization rate of the poplar alkali extract in step (3) of Example 1 is 82.9 ± 0.07%.

[0082] Comparative Example 1

[0083] A method for purifying poplar alkali: (1) Grind poplar alkali into powder with a pulverizer, pass through a 60-mesh sieve to obtain poplar alkali powder. Mix the poplar alkali powder with ultrapure water and perform ultrasonic extraction. The mass ratio of poplar alkali powder to the volume of ultrapure water is 1 g:40 mL. The temperature of ultrasonic extraction is 50 °C, the time of ultrasonic extraction is 15 min, and the power of ultrasonic extraction is 480 W. After ultrasonic extraction is completed, centrifuge at 5000 r / min for 10 min and perform vacuum filtration to obtain the original poplar alkali solution;

[0084] (2) Mix phosphorus-free activated carbon (Beijing Solarbio Science & Technology Co., Ltd., analytical pure) with the original solution of poplar alkali for decolorization treatment. The mass ratio of phosphorus-free activated carbon to the volume of the original solution of poplar alkali is 1 g:100 mL. The temperature of the decolorization treatment is 51 °C, the time is 82 min, and the pH value is 8.5. After the decolorization treatment is completed, centrifuge at 5000 r / min for 10 min and then perform vacuum filtration to obtain the poplar alkali extract.

[0085] Comparative Examples 2 - 5

[0086] Replace the mass ratio of phosphorus-free activated carbon to the volume of the poplar alkali extract in step (2) of Comparative Example 1 with 2 g:100 mL, 3 g:100 mL, 4 g:100 mL, and 5 g:100 mL respectively, and keep other parameters the same as those in Comparative Example 1 to obtain the poplar alkali extract.

[0087] The macroscopic view of the poplar alkali extract obtained in step (3) of Example 1 is as Figure 1 shown.

[0088] The macroscopic views of the poplar alkali extracts obtained in Comparative Examples 1 - 5 are as Figure 2 shown. Figure 2 From left to right are Comparative Examples 1 - 5 in Figures 1-2 It can be seen that when using activated carbon without alkali treatment and acid treatment for decolorization, the color of the poplar alkali extract cannot be removed and it contains black substances, while when using activated carbon treated with alkali and acid for decolorization, the color of the poplar alkali extract is basically removed and it does not contain black substances.

[0089] In summary, in the present invention, the activated carbon is sequentially treated with alkali and acid to obtain activated activated carbon, and then the activated activated carbon is used to decolorize the original solution of poplar alkali, removing the impurities in the original solution of poplar alkali and improving the decolorization rate.

[0090] The above are only the preferred embodiments of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.

Claims

1. A method for purifying populin, comprising the following steps: (1) Mix populin with water and perform ultrasonic extraction to obtain a crude populin solution; (2) Mix activated carbon with an alkali solution and perform alkali treatment to obtain alkali-treated activated carbon; (3) Mix the alkali-treated activated carbon obtained in step (2) with an acid solution and perform acid treatment to obtain activated activated carbon; (4) Mix the crude populin solution obtained in step (1) and the activated activated carbon obtained in step (3) and perform decolorization treatment to obtain a populin extract; There is no order of priority between step (1) and steps (2)-(3).

2. The purification method according to claim 1, characterized in that, The particle size of populin in step (1) is ≤60 mesh.

3. The purification method according to claim 1, wherein The mass ratio of populin to the volume of water in step (1) is 1 g:(35-45) mL.

4. The purification method according to claim 1, characterized in that, In step (1), the temperature of ultrasonic extraction is 45-55°C, the time of ultrasonic extraction is 10-20 min, and the power of ultrasonic extraction is 420-540 W.

5. The purification method according to claim 1, wherein In step (2), the mass concentration of the alkali solution is 3-7%.

6. The purification method according to claim 1, wherein In step (2), the time of alkali treatment is 20-30 min.

7. The purification method according to claim 1, wherein In step (3), the concentration of the acid solution is 4-8 mol / L.

8. The purification method according to claim 1, characterized in that, In step (3), the time of acid treatment is 20-30 min.

9. The purification method according to claim 1, wherein In step (4), the mass ratio of activated activated carbon to the volume of the crude populin solution is (5-5.5) g:100 mL.

10. The purification method according to claim 1, characterized in that, In step (4), the temperature of decolorization treatment is 50-55°C, the time of decolorization treatment is 80-85 min, and the pH value of decolorization treatment is 8-9.

Images