CN114573836A - Hydrogel and method for producing same - Google Patents
Hydrogel and method for producing same Download PDFInfo
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- CN114573836A CN114573836A CN202210215389.6A CN202210215389A CN114573836A CN 114573836 A CN114573836 A CN 114573836A CN 202210215389 A CN202210215389 A CN 202210215389A CN 114573836 A CN114573836 A CN 114573836A
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 49
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 27
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 66
- 150000001875 compounds Chemical class 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 21
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 20
- 229920002678 cellulose Polymers 0.000 claims abstract description 19
- 239000001913 cellulose Substances 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 239000008247 solid mixture Substances 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000007790 solid phase Substances 0.000 claims abstract description 8
- 150000002334 glycols Chemical class 0.000 claims abstract description 7
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims description 34
- 238000004132 cross linking Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 239000008213 purified water Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000000084 colloidal system Substances 0.000 claims description 5
- 239000012043 crude product Substances 0.000 claims description 5
- 229940057838 polyethylene glycol 4000 Drugs 0.000 claims description 5
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 239000000499 gel Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 4
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 4
- 238000003892 spreading Methods 0.000 claims description 4
- 230000007480 spreading Effects 0.000 claims description 4
- 229940093429 polyethylene glycol 6000 Drugs 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000003431 cross linking reagent Substances 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 3
- 229960004106 citric acid Drugs 0.000 description 17
- 239000002245 particle Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 239000007787 solid Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 4
- 239000008194 pharmaceutical composition Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 208000008589 Obesity Diseases 0.000 description 3
- 206010012601 diabetes mellitus Diseases 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 230000002641 glycemic effect Effects 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 235000020824 obesity Nutrition 0.000 description 3
- 230000036186 satiety Effects 0.000 description 3
- 235000019627 satiety Nutrition 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000004260 weight control Methods 0.000 description 3
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 description 2
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 229960002303 citric acid monohydrate Drugs 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000600 sorbitol Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000019577 caloric intake Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000012674 dispersion polymerization Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 235000012631 food intake Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000005414 inactive ingredient Substances 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- -1 solubilization Substances 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/26—Cellulose ethers
- C08J2301/28—Alkyl ethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/092—Polycarboxylic acids
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Medicinal Preparation (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention relates to the field of preparation of hydrogel, and particularly relates to hydrogel and a production method thereof. The production method of the hydrogel comprises the following steps: mixing water, polyethylene glycol compound, citric acid and cellulose compound, grinding to obtain completely molten semi-solid mixture, and performing solid phase polymerization. Citric acid is used as a cross-linking agent, polyethylene glycol compounds are used as an auxiliary cross-linking agent, and the mixing mode for preparing the hydrogel is changed from solution mixing to semi-solid phase mixing, so that the production time is shortened, and the production efficiency is greatly improved; the method has the advantages of reducing the using amount of water, saving energy, protecting environment, improving the performance of the prepared hydrogel, improving the medium intake ratio and not obviously reducing the elastic modulus.
Description
Technical Field
The invention relates to the field of hydrogel preparation, and particularly relates to hydrogel and a production method thereof.
Background
Hydrogels (hydrogels) are a class of very hydrophilic three-dimensional network-structured gels that swell rapidly in water and in this swollen state can hold a large volume of water without dissolving. In the prior art, a fiber compound is generally used as a substrate to react with a cross-linking agent so as to prepare hydrogel. In addition, in the preparation process, citric acid is usually used as a cross-linking agent, and the solution dispersion polymerization is carried out in the form of an aqueous solution in the reaction system, but the solubility of the fiber compound is low, so that the concentration of the fiber compound is usually 4-6% relative to the weight of water. The dissolution rate is very slow, typically requiring tens of hours; and the water solvent needs to be removed at a later stage, so that a large amount of energy consumption is required. And the performance of the hydrogel prepared by the crosslinking agent and the method is not particularly excellent.
Disclosure of Invention
The present invention provides a hydrogel and a method for producing the same, aiming at improving the above problems.
The invention is realized by the following steps:
in a first aspect, an embodiment of the present invention provides a method for producing a hydrogel, including: mixing water, polyethylene glycol compound, citric acid and cellulose compound, grinding to obtain completely molten semi-solid mixture, and performing solid phase polymerization.
Further, in a preferred embodiment of the present invention, the method comprises: mixing purified water, citric acid and polyethylene glycol compounds at 20-60 deg.C, stirring for dissolving, slowly and uniformly adding cellulose compounds into the above solution, stirring, and grinding with colloid mill to obtain completely dissolved semisolid mixture.
Further, in a preferred embodiment of the present invention, the mass ratio of the water, the citric acid, the polyethylene glycol compound and the cellulose compound is 6-12: 0.008-0.012: 0.08-0.14: 1.
further, in a preferred embodiment of the present invention, the cellulose-based compound comprises sodium carboxymethyl cellulose.
Further, in a preferred embodiment of the present invention, the polyethylene glycol compounds include polyethylene glycol 4000 and polyethylene glycol 6000.
Further, in a preferred embodiment of the present invention, the solid-phase polymerization comprises: drying the semi-solid mixture at 40-100 ℃ until the loss on drying is not more than 15%, and then carrying out crosslinking reaction at 100-140 ℃.
Further, in a preferred embodiment of the present invention, the production method further comprises: spreading the semi-solid mixture in a baking pan, drying at 40-100 ℃ until the loss on drying is not more than 15%, crushing, crosslinking at 100-140 ℃ for 3-4 hours to form a crosslinked crude product, and cleaning and drying.
Further, in the preferred embodiment of the present invention, the diameter of the pulverized material is 100-1000 microns.
Further, in a preferred embodiment of the present invention, the drying process comprises: drying at 65-85 deg.C for 24-30 hr, and drying at 40-50 deg.C until the loss on drying is less than 10%.
In a second aspect, embodiments of the present invention provide a hydrogel prepared by the above-described method for producing a hydrogel.
The invention has the beneficial effects that: according to the embodiment of the invention, citric acid is used as a cross-linking agent, polyethylene glycol compounds are used as an auxiliary cross-linking agent, and the mixing mode for preparing hydrogel is changed from solution mixing to semi-solid phase mixing, so that the production time is shortened, and the production efficiency is greatly improved; the method has the advantages of reducing the using amount of water, saving energy, protecting environment, improving the performance of the prepared hydrogel, improving the medium intake ratio and not obviously reducing the elastic modulus.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following provides a detailed description of a hydrogel and a method for producing the same.
First, the present invention provides a method for producing a hydrogel, comprising:
mixing water, polyethylene glycol compound, citric acid and cellulose compound, grinding to obtain completely molten semi-solid mixture, and performing solid phase polymerization. In particular, the amount of the solvent to be used,
adding purified water, citric acid and polyethylene glycol compounds into a low-shear normal-pressure mixing container at 20-60 deg.C, stirring to dissolve to form a solution, slowly and uniformly adding cellulose compounds into the above solution, and stirring for 15-30min to uniformly disperse cellulose compounds in water without obvious large agglomerates or powdery materials. The mixture is then poured into a colloid mill and milled using the colloid mill multiple times (e.g., 2 times) to obtain a fully melted semi-solid mixture.
The completely melted semi-solid mixture is: the cellulose compound and the water are completely bonded, and the solid-liquid separation phenomenon does not exist between the cellulose compound and the water; the semi-solid mixture is in a uniform state, and the surface is flat and smooth; the color is nearly colorless and transparent, and no granular objects exist.
The cellulose compound can be the known cellulose compound in the prior art, and the sodium carboxymethyl cellulose is selected in the embodiment of the invention because the sodium carboxymethyl cellulose has high water solubility, so that the water consumption can be properly reduced, and the semi-solid mixing formation can be promoted.
The polyethylene glycol compounds may be polyethylene glycols known in the art, such as polyethylene glycol 4000 and polyethylene glycol 6000.
The citric acid used is citric acid monohydrate, and non-hydrated citric acid can also be used.
The mass ratio of the water to the citric acid to the polyethylene glycol compound to the cellulose compound is 6-12: 0.008-0.012: 0.08-0.14: 1. by adopting the proportion, the performance of the formed hydrogel can be better improved, and the elastic modulus is not obviously reduced while the medium intake ratio is improved.
Then spreading the completely melted semi-solid mixture into a stainless steel baking pan (the thickness is not more than 30mm), and then placing the semi-solid mixture into an oven for drying, specifically, drying for 30-40h at 40-100 ℃, for example, at any value of 40-100 ℃ such as 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃ and 100 ℃, and drying for 30-40h such as 30h, 31h, 32h, 33h, 34h, 35h, 36h, 37h, 38h, 39h and 40 h. And the weight loss on drying is not more than 15 percent, and the middle part is overturned once.
And then crushing the hard and brittle solid obtained by drying, specifically, cutting the hard and brittle solid into small pieces of about 5cm by using a coarse grinding machine, crushing by using a fine grinding machine, and sieving to collect particles with the diameter of 100-1000 microns (20-150 meshes).
Then, the particles obtained by the above pulverization are placed into a crosslinking reactor, and are placed at any value between 100-140 ℃ such as 100 ℃, 105 ℃, 110 ℃, 115 ℃, 120 ℃, 125 ℃, 130 ℃, 135 ℃ and 140 ℃ to carry out crosslinking reaction for about 3-4h, for example, any value between 3-4h such as 3h, 3.5h and 4h, and obtain a crosslinked crude product.
The crosslinked crude product was transferred to a washing tank, washed with 150-fold 200-fold purified water to remove by-products and unreacted raw materials, and filtered. The filtered solid is placed in a tray for ventilation drying, the thickness is 40mm, and the solid is dried at 65-85 ℃ for 24-30 hours, for example, the drying temperature is 65 ℃, 66 ℃, 67 ℃, 68 ℃, 69 ℃, 70 ℃, 71 ℃, 72 ℃, 73 ℃, 74 ℃, 75 ℃, 76 ℃, 77 ℃, 78 ℃, 79 ℃, 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃ and 85 ℃ at any value between 65-85 ℃, and the drying time is 24 hours, 25 hours, 26 hours, 27 hours, 28 hours, 29 hours, 30 hours and other values between 24-30 hours. Then dried at 40-50 ℃ until the loss on drying is < 10%. For example, the temperature is any value between 40-50 ℃ such as 40 ℃, 41 ℃, 42 ℃, 43 ℃, 44 ℃, 45 ℃, 46 ℃, 47 ℃, 48 ℃, 49 ℃ and 50 ℃. And then granulating, and collecting 20-150 mesh granules.
The embodiment of the invention provides a hydrogel which is prepared by the production method of the hydrogel.
The hydrogels of the present invention may be used in methods of treating obesity, reducing food or calorie intake, or achieving or maintaining satiety. The hydrogels of the present invention may also be used to improve glycemic control, treat or prevent diabetes, or aid in weight control. The product can be taken alone, or taken with liquid or food.
The hydrogels of the present invention may be used as pharmaceutical compositions that may include the hydrogel as an active ingredient, optionally in combination with pharmaceutically acceptable excipients or carriers. The pharmaceutical composition may be suitable for oral administration to treat obesity, enhance satiety, improve glycemic control, treat or prevent diabetes, or aid in weight control.
The hydrogel can be used as a pharmaceutical composition, wherein the hydrogel is used as an inactive ingredient, plays roles of slow release, dispersion, solubilization, coating and the like in the composition, and is suitable for different action purposes. The pharmaceutical composition may be suitable for oral administration to treat obesity, enhance satiety, improve glycemic control, treat or prevent diabetes, or aid in weight control.
The related detection of the hydrogel provided by the embodiment of the invention comprises yield, medium uptake ratio, elastic modulus, water content and tap density. The detection method of each item is as follows:
firstly, a method for measuring tap density (DT, g/ml):
accurately weighing 40.0 + -0.1 g of test particles (M, g), pouring into a dry 100ml graduated glass cylinder, shaking or tapping the cylinder until the readings do not change (the difference between 2 readings is less than 2%), and recording the final vibrating volume (V)f，ml)。
DT＝M/Vf。
Second, a method for measuring a Medium Uptake Ratio (MUR):
the 6 dried sintered glass funnels were washed clean with 40ml of purified water, placed on a stand, the funnel blotted dry with filter paper, weighed, and the weight of the empty device (W) recordedtare)。
Accurately weighing 0.250 + -0.005 g of test particles (W)in) The mixture was put into a 100ml beaker, and 40.0. + -. 0.1g of purified water was added thereto, and the mixture was gently shaken to obtain a suspension, and the suspension was gently stirred for 30 minutes to obtain a suspension. The suspension was poured into a funnel, drained for 10 minutes until no water drops were present, blotted dry with filter paper and weighed accurately to 0.1g (W)fin)。MUR＝(Wfin-Wtare-Win)/Win. Parallel to 3 portions, take the average.
Third, modulus of elasticity
And detecting by using an extensometer, paralleling by 3 parts, and taking an average value.
The following will specifically explain a hydrogel and a method for producing the same according to the present invention with reference to specific examples.
Examples 1 to 4
Examples 1 to 4 and comparative examples 1 to 5 were substantially the same except that the mass ratio of the polyethylene glycol-based compound, the citric acid and the cellulose-based compound was different, and the specific operation was as follows:
(1) adding 300kg of purified water, 300g of citric acid monohydrate and Xkg polyethylene glycol 4000 (the specific dosage is shown in table 1) into a low-shear normal-pressure mixing container at the temperature of 40 ℃, stirring and dissolving, slowly and uniformly adding 30kg of CMC-Na into the solution, and stirring for 15min to ensure that the CMC-Na is uniformly dispersed in the water and has no obvious large bulk or powdery materials. Pouring the mixture into a colloid mill at 2900r/min, and grinding for 2 times to obtain completely melted semisolid mixture.
(2) Spreading the completely melted semi-solid mixture into a stainless steel baking pan (thickness not more than 30 mm);
(3) drying in an oven at 80 deg.C for 40 hr until the loss of drying is not more than 15%, and turning over once in the middle.
(4) And shearing the hard and brittle solid obtained by drying into small pieces of about 5cm by using a coarse grinding machine, crushing by using a fine grinding machine, sieving, and collecting particles with the diameter of 100-1000 microns (20-150 meshes).
(5) And (3) putting the crushed particles into a crosslinking reactor, putting the crosslinking reactor into a drying oven at 140 ℃ for crosslinking reaction for about 3 hours to obtain the crude crosslinked cellulose particles.
(6) Transferring the crude product particles to a washing tank, washing with 200 times of purified water to remove by-products and unreacted raw materials, and filtering; the solid obtained by filtration was put on a tray and air-dried to a thickness of 40mm, and dried at 85 ℃ for 28 hours. Then drying at 50 ℃ until the loss on drying is less than 10 percent and the total drying time is about 60 hours; and (4) finishing the granules, collecting 20-150-mesh granules, and weighing Zkg.
Calculating the yield: z/30 x 100%.
Comparative example 6: the hydrogel was prepared by referring to the production method of the above example except that polyethylene glycol 4000 was replaced with sorbitol in an equimolar amount to example 1.
Then, the hydrogels prepared in the examples and comparative examples were tested, and the test results are shown in table 1.
TABLE 1
According to the above table, when only citric acid is used as the crosslinking agent, i.e. comparative example 1, the medium uptake ratio of the formed hydrogel is only 32MUR, and the elastic modulus is 1.62Kpa, but when citric acid and polyethylene glycol are used for matching, the medium uptake ratio is improved, the elastic modulus is not obviously reduced, and the performance of the formed hydrogel is improved. If the proportion of the citric acid and the polyethylene glycol is within the range defined by the invention, the hydrogel has higher medium uptake ratio under the condition of not obviously reducing the elastic modulus of the hydrogel, and the performance is further improved. If the combination of citric acid and polyethylene glycol as the cross-linking agent is changed, for example, the combination of citric acid and sorbitol is changed, the yield of the hydrogel is greatly reduced, and the medium uptake ratio is also lower than 50MUR, which indicates that the performance of the hydrogel is reduced. Further verifies that the performance of the hydrogel can be effectively improved by specifically matching citric acid and polyethylene glycol.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method of producing a hydrogel, comprising: mixing water, polyethylene glycol compound, citric acid and cellulose compound, grinding to obtain completely molten semi-solid mixture, and performing solid phase polymerization.
2. The method for producing a hydrogel according to claim 1, comprising: mixing purified water, citric acid and polyethylene glycol compounds at 20-60 deg.C, stirring for dissolving, slowly and uniformly adding cellulose compounds into the above solution, stirring, and grinding with colloid mill to obtain completely dissolved semisolid mixture.
3. The method for producing a hydrogel according to claim 1, wherein the mass ratio of the water, the citric acid, the polyethylene glycol-based compound, and the cellulose-based compound is 6 to 12: 0.008-0.012: 0.08-0.14: 1.
4. the method for producing a hydrous gel according to any one of claims 1 to 3, wherein said cellulose-based compound comprises sodium carboxymethylcellulose.
5. The method for producing a hydrous gel as claimed in any one of claims 1 to 3, wherein said polyethylene glycol-based compound comprises polyethylene glycol 4000 and polyethylene glycol 6000.
6. The method for producing a hydrogel according to claim 1, wherein the solid-phase polymerization comprises: drying the semi-solid mixture at 40-100 ℃ until the loss on drying is not more than 15%, and then carrying out crosslinking reaction at 100-140 ℃.
7. The method for producing a hydrogel according to claim 6, further comprising: spreading the semi-solid mixture in a baking pan, drying at 40-100 ℃ until the loss on drying is not more than 15%, crushing, crosslinking at 100-140 ℃ for 3-4 hours to form a crosslinked crude product, and cleaning and drying.
8. The method for producing a hydrous gel as claimed in claim 7, wherein the diameter of the pulverized material is 100-1000 μm.
9. The method for producing a hydrogel according to claim 7, wherein the drying process comprises: drying at 65-85 deg.C for 24-30 hr, and drying at 40-50 deg.C until the loss on drying is less than 10%.
10. A hydrogel produced by the method for producing a hydrogel according to any one of claims 1 to 9.
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