Resin column purification device for mirabilitum praeparatum toothpaste production

Abstract

The utility model provides a resin column purification device for mirabilitum praeparatum toothpaste production. The resin column purification device comprises an extracting solution storage tank, a tubular centrifuge and a chromatographic separation device which are connected in sequence, and water eluent and alcohol eluent output by the chromatographic separation device are respectively introduced into a theanine purification section and a tea polyphenol purification section to obtain purified theanine and tea polyphenol; the theanine purification section comprises a first mixing tank, a cation exchange resin column and a first concentrator which are connected in sequence, output liquid of the acid liquor storage tank is connected into the first mixing tank, and output liquid of the alkali liquor storage tank is connected into the cation exchange resin column; the tea polyphenol purification section comprises a desorption solution storage tank and a second concentrator which are connected in sequence. The resin column purification device for mirabilitum praeparatum toothpaste production provided by the utility model can effectively separate and purify amino acid and tea polyphenol in a tea extract, and improves the treatment capacity of a tea extracting solution.

Description

TECHNICAL FIELD

[0001] The utility model relates to the technical field of extraction equipment, concretely is a resin column purification device for watermelon frost toothpaste production. BACKGROUND

[0002] In recent years, in the oral care field, tea toothpaste and mouthwash are deeply loved by consumers because of their excellent health care function and unique taste, and their market share in oral care is increasing year by year. The main organic compounds in tea are tea polyphenols, alkaloids, sugars and amino acids, and the main inorganic compounds are potassium, sodium, magnesium and fluorine. Tea extract is a solution or powder obtained by extracting, filtering, distilling, purifying and concentrating tea leaves with hot water or ethanol as solvent, which contains higher content of functional ingredients such as tea polyphenols, amino acids and active fluorine.

[0003] Tea polyphenols are a complex of various polyhydroxy phenolic compounds, including catechins, flavones, flavonols, phenolic acid, phenolic acid and anthocyanins, etc., among which catechins account for 60-80% of the total mass of tea polyphenols. Currently, tea polyphenols are generally extracted from tea leaves, and among all tea types, green tea contains the highest content of tea polyphenols, about 15-30% of the mass of green tea. Tea polyphenols have the effects of inhibiting the growth of dental plaque, promoting the remineralization of early caries, blocking exposed dental tubules, and effectively resisting dental acid erosion. In addition, tea polyphenols can effectively remove oral odor, freshen breath, and help reduce the damage of free radicals to the gums and oral cavity.

[0004] Theanine is a characteristic amino acid of tea leaves, and is the main flavoring substance that gives tea extract a caramel-like and umami-like fresh taste. As a food additive, it is favored by consumers due to its good taste, safety, stability and no toxic side effects. Theanine is easily soluble in water, can inhibit bitterness and improve food flavor, can effectively improve the bitter taste of tea polyphenols, and can give oral cleaning and refreshing unique experience when added to tea toothpaste and mouthwash.

[0005] Currently, the preparation methods of tea extract generally include biological fermentation method, chemical synthesis method, chemical extraction method and column chromatography method. Theanine extracted by biological fermentation method is expensive; the safety of chemically synthesized theanine and tea polyphenols needs to be verified. The chemical extraction method mainly includes ion precipitation method, organic solvent extraction method and chromatography method. The ion precipitation method uses chloroform and introduces harmful heavy metal Pb 2+ There are obvious deficiencies in the extraction of natural theanine; in the organic solvent extraction method, caffeine and tea polysaccharides have multiple functions and are difficult to separate from tea polyphenols, and the impurity content in the final product is high. The resin chromatography method for separating tea polyphenols and theanine has less impurities and less environmental pollution, and has development and application prospect.

[0006] But now there is no effective market access tea polyphenols, amino acid resin chromatography purification equipment, to ensure the quality of tea polyphenols, amino acid extraction to be applied to the production of watermelon frost toothpaste, need to design a resin column purification device for watermelon frost toothpaste production. The utility model discloses a resin column purification device for watermelon frost toothpaste production

[0007] The utility model provides a resin column purification device for watermelon frost toothpaste production can separate and purify amino acid, tea polyphenols in tea extract, obtain the tea extract that satisfies watermelon frost toothpaste production, can improve the processing capacity and production efficiency of tea extract.

[0008] To realize above-mentioned technical purpose, reach above-mentioned technical effect, the utility model solves above-mentioned problem through following technical scheme:

[0009] A resin column purification device for watermelon frost toothpaste production, including the extraction liquid storage tank, tubular centrifuge that connect in turn, chromatographic separation device, and the water eluent, alcohol eluent of chromatographic separation device output respectively access tea amino acid purification section and tea polyphenols purification section, the tea amino acid purification section includes the first mixing tank, cation exchange resin column, first concentrator that connect in turn, and the acid liquid storage tank output liquid accesses the first mixing tank, and the lye storage tank output liquid accesses cation exchange resin column, the tea polyphenols purification section includes the analytical liquid storage tank, second concentrator that connect in turn, the concentrated liquid of first concentrator and second concentrator is output to the second mixing tank mixing, and the second mixing tank is connected spray drying tower.

[0010] Further, the chromatographic separation device includes a plurality of macroporous adsorption resin columns connected in parallel to form a chromatographic column group, each macroporous adsorption resin column is connected to a feed pipe at the top through a pipe and an upper column valve, and the head of the feed pipe is connected to the tubular centrifuge through a feed valve; an alcohol liquid storage tank is connected to the feed pipe through an alcohol delivery pump and an alcohol liquid valve, and a water liquid storage tank is connected to the feed pipe through a water delivery pump and a water liquid valve; each macroporous adsorption resin column is provided with a lower column valve at the bottom, and the lower column valve is connected to a water eluent discharge pipe and an alcohol eluent discharge pipe through a lower column pipe; the water eluent discharge pipe is connected to the first mixing tank through a mixer front valve; and the alcohol eluent discharge pipe is connected to the analytical liquid storage tank through an alcohol eluent discharge valve and an ultraviolet detector.

[0011] Further, the water eluent discharge pipe is connected to the water delivery pump output end through an activation water inlet valve at the front end, the tail of the feed pipe serves as an activated water discharge end, and an activated backwash water is discharged through an activated drain valve; a water washing communication valve is arranged between the water eluent discharge pipe and adjacent two lower column pipes; and the lower column pipe is connected to the alcohol eluent discharge pipe through an alcohol washing communication valve.

[0012] Further, the water eluent discharge pipe is connected to a water washing emptying pipeline through a tee joint at the front side of the mixer front valve, and an emptying valve is arranged to control the opening and closing of the water washing emptying pipeline.

[0013] Further, the macroporous adsorption resin column in the chromatographic separation device is 6, and the height-diameter ratio of the macroporous adsorption resin column is 1-4:1.

[0014] Further, the alcohol liquid in the alcohol liquid storage tank is 60-80% ethanol.

[0015] Further, the cation exchange resin column is a macroporous cation exchange resin column, the height-diameter ratio of the cation exchange resin column is 1-4:1, and the volume-mass ratio (L / Kg) of the cation exchange resin column to the tea raw material is 0.2-0.6:1.

[0016] Further, the acid liquid in the acid liquid storage tank is 0.5-2 mol / L hydrochloric acid, and the dilute alkali liquid in the alkali liquid storage tank is 1-2 mol / L ammonia water solution.

[0017] Further, the elution liquid storage tank is provided with an elution liquid emptying pipeline at the bottom, and an elution tank lower valve is configured to control the on-off.

[0018] The advantages and effects of the utility model are:

[0019] 1. The scheme is used for separating theanine and tea polyphenols in tea extract, after the tea extract is impurity-removed by a tubular centrifuge, the tea extract is sequentially subjected to water elution and alcohol elution in a chromatographic separation device. The water elution liquid is subjected to acid conversion, and then is further impurity-removed by a cation ion exchange resin, and after being eluted by a weak alkali ammonia test solution, high-purity theanine is obtained by concentration and drying; the alcohol elution liquid is eluted, concentrated and dried to obtain high-purity tea polyphenols. The device can effectively improve the processing capacity of the tea extract and achieve large-scale production.

[0020] 2. The macroporous adsorption resin column of the chromatographic separation device can share a discharge port to realize water washing and alcohol washing, and can realize the control selection of elution and backwashing through the switching control of the valve. The backwashing can effectively activate the water washing of the resin, improve the regeneration efficiency of the resin, reduce the operation difficulty and effectively control the use amount of the material and the activating reagent. At the same time, the valve control can realize single control and multi-control parallel resin columns, which is more convenient and reasonable in actual application.

[0021] 3. The scheme sets the cation ion exchange resin to further impurity-remove the solution, and the color of the water-soluble impurities which are relatively deep is obviously lighter after passing through the cation exchange column, which better meets the requirements of toothpaste and mouthwash preparations, improves the experience of the products and avoids the generation of solid waste and the significant loss of functional components caused by the use of activated carbon for impurity removal. BRIEF DESCRIPTION OF DRAWINGS

[0022] Figure 1 The figure is a structural schematic view of the utility model;

[0023] Figure 2 The figure is a structural schematic view of the chromatographic separation device in the utility model.

[0024] Figure number identification:

[0025] 1, extraction tank, 2, tubular centrifuge, 3, chromatographic separation device, 4, the first mixing tank, 5, cation exchange resin column, 6, the first concentrator, 7, acid liquid storage tank, 8, alkali liquid storage tank, 9, eluent tank, 10, the second concentrator, 11, the second mixing tank, 12, spray drying tower, 13, elution tank valve, 14, effluent valve; 15, infusion pump I, 16, infusion pump II, 17, infusion pump III, 18, infusion pump IV, 19, cation column valve;

[0026] 301, macroporous adsorption resin column, 302, column valve, 303, feed pipe, 304, feed valve, 305, alcohol liquid storage tank, 306, alcohol pump, 307, alcohol pipe valve, 308, water liquid storage tank, 309, water pump, 310, water pipe valve, 311, column valve, 312, column pipe, 313, water washing liquid discharge pipe, 314, alcohol washing liquid discharge pipe, 315, mixer front valve, 316, alcohol washing discharge valve, 317, ultraviolet detector, 318, activation water valve, 319, emptying valve, 320, water washing communication valve, 321, alcohol washing communication valve, 322, activation drain valve, 323, feed intermediate valve. DETAILED DESCRIPTION

[0027] The utility model will be further described below in combination with examples, but the utility model is not limited to these examples.

[0028] The resin column purification device for watermelon frost toothpaste production described in this example, as shown in the accompanying drawings, comprises extraction tank 1, infusion pump I 15, tubular centrifuge 2, chromatographic separation device 3 connected in sequence through pipelines, wherein chromatographic separation device 3 has two discharge pipelines of water washing liquid discharge pipe 313 and alcohol washing liquid discharge pipe 314, the water washing eluent discharged from water washing liquid discharge pipe 313 is connected to the tea amino acid purification section, and the alcohol washing eluent discharged from alcohol washing liquid discharge pipe 314 is connected to the tea polyphenol purification section. Figure 1 The tea amino acid purification section comprises first mixing tank 4, infusion pump II 16, cation column valve 19, cation exchange resin column 5 and first concentrator 6 connected in sequence, the output liquid of acid liquid storage tank 7 is connected to first mixing tank 4 through acid liquid valve, and the output liquid of alkali liquid storage tank 8 is connected to cation exchange resin column 5 through alkali liquid valve, wherein the bottom of cation exchange resin column 5 is provided with effluent pipeline, and effluent valve 14 is configured to control the on-off.

[0029]

[0030] ​The tea polyphenol purification section includes a sequentially connected analytical solution storage tank 9, a second concentrator 10, and an infusion pump III 17. The output of the infusion pump III is connected to a second mixing tank 11, which mixes theanine and purified tea polyphenol solution and delivers it to a spray drying tower 12 via an infusion pump IV 18. A analytical solution drain line is located at the bottom of the analytical solution storage tank 9, and a lower valve 13 is provided to control the on / off operation of the analytical solution.

[0031] As attached Figure 2 As shown, the chromatographic separation device 3 includes a chromatographic column assembly consisting of six macroporous adsorbent resin columns 301 connected in parallel. The top of each macroporous adsorbent resin column 301 is connected to a feed pipe 303 via a pipe and a column valve 302. The head of the feed pipe 303 is connected to the tubular centrifuge 2 via a feed valve 304. An alcohol storage tank 305 is connected to the feed pipe 303 via a pipe via an alcohol pump 306 and an alcohol pipe valve 307. A water storage tank 308 is connected to the feed pipe 303 via a pipe via a water pump 309 and a water pipe valve 310. To avoid waste and improve control accuracy, in this embodiment, an intermediate feed valve 323 is added to the feed pipe 303 behind the feed valve 304. The alcohol and water liquids are connected to the front and back sides of the intermediate feed valve 323, respectively.

[0032] The bottom of each macroporous adsorption resin column 301 is connected to a column downpipe 312 and is equipped with a column downpipe valve 311. The column downpipe 312 is connected to a water wash liquid discharge pipe 313, which is then connected to an alcohol wash liquid discharge pipe 314 via an alcohol wash connecting valve 321. The water wash liquid discharge pipe 313 is connected to the first mixing tank 4 via a mixer pre-valve 315. In front of the mixer pre-valve 315, the water wash liquid discharge pipe 313 is connected to a water wash drain line via a tee, and a drain valve 319 is provided to control its on / off. The tail end of the alcohol wash liquid discharge pipe 314 is connected to the analytical solution storage tank 9 via an alcohol wash discharge valve 316 and a UV detector 317.

[0033] To achieve backwashing, the front end of the wash liquid discharge pipe 313 is connected to the output of the water pump 309 via an activated water inlet valve 318. The tail end of the feed pipe 303 serves as the activated water discharge end, and the discharge of activated backwash water is controlled by an activated drain valve 322. A water wash connecting valve 320 is installed between the wash liquid discharge pipe 313 and the connection point between it and the two adjacent column downpipes 312.

[0034] The acid solution in the acid storage tank 7 is 0.5-2 mol / L hydrochloric acid, preferably 1.0 mol / L in the embodiment. The test solution in the first mixing tank 4 is adjusted to a pH of 2.0-5.0 with the hydrochloric acid solution, preferably 3.0 in the embodiment. The dilute alkali solution in the alkali storage tank 8 is 1-2 mol / L ammonia solution, preferably 1.5 mol / L in the embodiment. The alcohol eluent in the alcohol storage tank 305 is 60-80% ethanol, preferably 1.5 mol / L in the embodiment.

[0035] The ratio of height to diameter of the macroporous adsorption resin column 301 in the chromatographic separation device 3 is 1-4:1, and the type of the macroporous adsorption resin column 301 is one or more of AB-8, D101, XDA-5, HPD600 or DM130. The cation exchange resin column 5 is a macroporous cation exchange resin column with a height to diameter ratio of 1-4, the volume to mass ratio (L / Kg) of the cation exchange resin column 5 to the tea raw material is 0.2-0.6:1, and the type of the cation exchange resin is one or more of 732, 724, 717, D945, and the preferred type in the embodiment is 732 macroporous cation exchange resin.

[0036] When the watermelon cream toothpaste production resin column purification device described in the embodiment is used:

[0037] The tea extract in the extract tank 1 is input into the tubular centrifuge 2 through the liquid pump I 15, and the centrifuged liquid is input into the chromatographic separation device 3. The centrifuged liquid is input into the feed pipe 303, and then slowly passes through the six resin columns 301 after passing through the feed valve 304, the feed intermediate valve 323, and the on-column valve 302, and is fully adsorbed. (The number of macroporous adsorption resin columns 301 used can be selected according to production needs, and the use of the on-column valve 323 and the under-column valve 311 is controlled to be on), and then the liquid is input into the alcohol washing liquid outlet pipe 314 through the under-column valve 311 and the alcohol washing communication valve 321. When the ultraviolet detector 317 detects a change in absorbance, the feed valve 304, the alcohol washing outlet valve 316, and the alcohol washing communication valve 321 are closed, and the mixer front valve 315, the water washing communication valve 320, and the water liquid valve 310 are opened for water washing and elution work. (At this time, all the valves in the chromatographic separation device 3 are closed.)

[0038] During the water washing and elution work, the drinking water in the water liquid tank 308 is input into the macroporous adsorption resin column 301 through the water pump 309, the water liquid valve 310, the feed pipe 303, and the on-column valve 302, and then the tea amino acid in the resin column is eluted. The water eluate is input into the first mixing tank 5 through the under-column valve 311, the water eluate outlet pipe 313, the water washing communication valve 320, and the mixer front valve 315, and then enters the tea amino acid purification section.

[0039] In the tea amino acid purification section, the acid liquid in the acid liquid tank 7 is input into the first mixing tank 4 through the acid liquid valve to mix with the water eluate to adjust the pH. After the acid is adjusted, the liquid is input into the cation exchange resin column 5 through the liquid pump II 16 and the cation column front valve 19 to be fully adsorbed. The alkali liquid in the alkali liquid tank 8 is input into the cation exchange resin column 5 through the alkali liquid valve to desorb the tea amino acid. The desorbed liquid is concentrated by the first concentrator 6 and then sent to the second mixer 10 for drying.

[0040] After the water elution work is completed, alcohol elution work is carried out, the cation column front valve 19, the water liquid pipe valve 310, the mixer front valve 315, the water washing communication valve 320 are closed, the alcohol liquid storage tank 305 is opened, the alcohol liquid pipe valve 307, the alcohol washing communication valve 321 are opened, the ethanol liquid in the alcohol liquid storage tank 305 is slowly passed through the macroporous adsorption resin column 301 through the column valve 302 to start elution to tea polyphenols. The alcohol elution liquid enters the alcohol elution liquid outlet pipe 314 through the column lower valve 311, the column lower pipe 312, the alcohol washing communication valve 321, when the ultraviolet detector 317 detects that the absorbance changes obviously, the resolving liquid lower valve 13 is closed, the alcohol elution liquid is collected in the resolving liquid storage tank 9, the alcohol elution liquid is concentrated through the second concentrator 10, is sent into the second mixing tank 11 through the liquid pump III 17, after the tea polyphenols, tea amino acid liquid are mixed uniformly, are sent into the spray drying tower 12 through the liquid pump IV 18, and the target tea extract is obtained after being sprayed and dried.

[0041] When the macroporous adsorption resin column 301 needs to be activated and backflushed, the water liquid pipe valve 310, the mixer front valve 315, the alcohol washing communication valve 321, the emptying valve 319, the feed intermediate valve 323 are in the closed state, the activation water inlet valve 318, the water washing communication valve 320, the column lower valve 311, the activation drainage valve 322 are opened, the water pump 309 is opened, the activation liquid can be passed through the activation water inlet valve 318, the water liquid discharge pipe 313, the column lower valve 311 to the macroporous adsorption resin column 301 to carry out backflushing and activation, the backflushing liquid is discharged through the feed pipe 313 tail activation drainage valve 322, and the activation efficiency can be effectively improved through the structure.

[0042] The embodiments of the utility model are described in detail in combination with the drawings, but the utility model is not limited to the described embodiments. For those skilled in the art, various changes, modifications, replacements and modifications of these embodiments without departing from the principles and spirits of the utility model still fall within the protection scope of the utility model.

Claims

1. A resin column purification device for watermelon frost toothpaste production, characterized by: The device comprises a extraction liquid tank (1), a tubular centrifuge (2) and a chromatographic separation device (3) connected in sequence, and the water eluent and alcohol eluent output by the chromatographic separation device (3) are connected to a theanine purification section and a tea polyphenol purification section respectively; The theanine purification section comprises a first mixing tank (4), a cation exchange resin column (5) and a first concentrator (6) connected in sequence, and the liquid output by an acid liquid storage tank (7) is connected to the first mixing tank (4) and the liquid output by an alkali liquid storage tank (8) is connected to the cation exchange resin column (5). The tea polyphenol purification section comprises a desorption liquid tank (9) and a second concentrator (10) connected in sequence, and the concentrated liquid output by the first concentrator (6) and the second concentrator (10) is mixed in a second mixing tank (11) and then connected to a spray drying tower (12).

2. The resin column purification device for watermelon frost toothpaste production according to claim 1, characterized in that: The chromatographic separation device (3) comprises a chromatographic column group composed of a plurality of macroporous adsorption resin columns (301) connected in parallel, the top of each macroporous adsorption resin column (301) is connected to a feed pipe (303) through a pipe and a column valve (302), the head of the feed pipe (303) is connected to the tubular centrifuge (2) through a feed valve (304), an alcohol liquid storage tank (305) is connected to the feed pipe (303) through an alcohol delivery pump (306) and an alcohol liquid pipe valve (307), and a water liquid storage tank (308) is connected to the feed pipe (303) through a water delivery pump (309) and a water liquid pipe valve (310). The bottom of each macroporous adsorption resin column (301) is provided with a column lower valve (311), the column lower valve (311) is connected to a water eluent discharge pipe (313) and an alcohol eluent discharge pipe (314) through a column lower pipe (312), the water eluent discharge pipe (313) is connected to the first mixing tank (4) through a mixer front valve (315), and the alcohol eluent discharge pipe (314) is connected to the desorption liquid tank (9) through an alcohol eluent discharge valve (316) and an ultraviolet detector (317).

3. The resin column purification device for watermelon frost toothpaste production according to claim 2, characterized in that: The front end of the water eluent discharge pipe (313) is connected to the output end of the water delivery pump (309) through an activation water inlet valve (318), and the tail of the feed pipe (303) is used as an activated water discharge end and is controlled by an activated water discharge valve (322). The water eluent discharge pipe (313) is provided with a water washing communication valve (320) between the connection points of the pipe and the adjacent two column lower pipes (312), and the column lower pipe (312) is connected to the alcohol eluent discharge pipe (314) through an alcohol washing communication valve (321).

4. The resin column purification device for watermelon frost toothpaste production according to claim 2, characterized in that: The water eluent discharge pipe (313) is connected to a water washing emptying pipe through a tee joint on the front side of the mixer front valve (315), and an emptying valve (319) is arranged to control the opening and closing of the pipe.

5. The resin column purification device for watermelon frost toothpaste production according to claim 2, characterized in that: The macroporous adsorption resin column (301) in the chromatographic separation device (3) is six, and the height-diameter ratio of the macroporous adsorption resin column (301) is 1-4:

1.

6. The resin column purification device for watermelon frost toothpaste production according to claim 2, characterized in that: The alcohol eluent in the alcohol liquid storage tank (305) is 60-80% ethanol.

7. The resin column purification device for watermelon frost toothpaste production according to claim 1, characterized in that: The cation exchange resin column (5) is a macroporous cation exchange resin column, the height-diameter ratio of the cation exchange resin column (5) is 1-4:1, and the volume-mass ratio of the cation exchange resin column (5) to tea raw materials is 0.2-0.6 L:1 Kg.

8. The resin column purification device for watermelon frost toothpaste production according to claim 1, characterized in that: The acid liquid in the acid liquid storage tank (7) is 0.5-2 mol / L hydrochloric acid; the dilute alkali liquid in the alkali liquid storage tank (8) is 1-2 mol / L ammonia water solution.

9. The resin column purification device for watermelon frost toothpaste production according to claim 1, characterized in that: The bottom of the resolving liquid storage tank (9) is provided with a resolving liquid emptying pipeline, and a resolving tank lower valve (13) is arranged to control the on-off.

Images