CN114262402B - Preparation method of macroporous adsorption resin for caramel decolorization - Google Patents
Preparation method of macroporous adsorption resin for caramel decolorization Download PDFInfo
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- 239000011347 resin Substances 0.000 title claims abstract description 81
- 229920005989 resin Polymers 0.000 title claims abstract description 81
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 66
- MIDXCONKKJTLDX-UHFFFAOYSA-N 3,5-dimethylcyclopentane-1,2-dione Chemical compound CC1CC(C)C(=O)C1=O MIDXCONKKJTLDX-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 235000013736 caramel Nutrition 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000004042 decolorization Methods 0.000 title claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000010438 heat treatment Methods 0.000 claims abstract description 34
- 239000004005 microsphere Substances 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 238000005406 washing Methods 0.000 claims abstract description 25
- 238000007265 chloromethylation reaction Methods 0.000 claims abstract description 20
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims abstract description 18
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 13
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- SAMJGBVVQUEMGC-UHFFFAOYSA-N 1-ethenoxy-2-(2-ethenoxyethoxy)ethane Chemical compound C=COCCOCCOC=C SAMJGBVVQUEMGC-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002841 Lewis acid Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 150000007517 lewis acids Chemical class 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 7
- 238000009835 boiling Methods 0.000 claims abstract description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 7
- 238000005086 pumping Methods 0.000 claims abstract description 7
- 238000007493 shaping process Methods 0.000 claims abstract description 7
- 239000011780 sodium chloride Substances 0.000 claims abstract description 7
- 239000003999 initiator Substances 0.000 claims abstract description 5
- 239000003054 catalyst Substances 0.000 claims abstract description 3
- 238000004090 dissolution Methods 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims abstract description 3
- 239000002184 metal Substances 0.000 claims abstract description 3
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 claims description 12
- 239000011592 zinc chloride Substances 0.000 claims description 9
- 235000005074 zinc chloride Nutrition 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 6
- HRQGCQVOJVTVLU-UHFFFAOYSA-N bis(chloromethyl) ether Chemical compound ClCOCCl HRQGCQVOJVTVLU-UHFFFAOYSA-N 0.000 claims description 6
- 239000003502 gasoline Substances 0.000 claims description 4
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 3
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 3
- 239000010413 mother solution Substances 0.000 claims description 2
- 239000012452 mother liquor Substances 0.000 abstract description 5
- 239000000049 pigment Substances 0.000 abstract description 4
- 238000004321 preservation Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 4
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 230000008961 swelling Effects 0.000 description 4
- 238000002845 discoloration Methods 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004218 chloromethyl group Chemical group [H]C([H])(Cl)* 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method of macroporous adsorption resin for caramel decoloration, which comprises the steps of preparing macroporous adsorption resin, adding polyvinyl alcohol into water for dissolution, adding sodium chloride, heating, adding styrene, diethylene glycol divinyl ether, divinylbenzene, an initiator and a pore-forming agent again, uniformly mixing, standing, stirring at a low speed, calling out spheres with required particle size, gradually heating in stages, carrying out heat preservation and shaping, washing out the pore-forming agent, and pumping out mother liquor to obtain the macroporous adsorption resin; chloromethylation is carried out on macroporous adsorption resin, and chloromethylation is carried out under the action of a metal catalyst to obtain chloromethylation microspheres; adding phenol, solvent and Lewis acid into chloromethylation microsphere, controlling the reaction temperature to be close to the boiling point of the solvent, and obtaining the adsorption resin with high specific surface area. The invention realizes the preparation of the resin with better mechanical strength and higher adsorption quantity, enhances the selectivity to the pigment in the caramel and has high-efficiency separability.
Description
Technical Field
The invention belongs to the technical field of resin preparation, and particularly relates to a preparation method of macroporous adsorption resin for caramel decolorization.
Background
At present, the decolourization of caramel is basically carried out by using wood activated carbon, and the decolourization rate can reach 120 percent. The wood activated carbon is in a powdery form of more than 90% due to the limitation of raw materials, can be widely applied to the field of medicine and food purification industry, but has the defect of low strength and is only disposable. The existing brands of macroporous adsorption resin, such as D101, AB103 and the like, are generally used for caramel decolorization effect, and can not meet the requirements of the caramel decolorization industry.
Disclosure of Invention
The invention aims to solve the technical problems and provide a preparation method of macroporous adsorption resin for caramel decolorization, so that the preparation of the resin with better mechanical strength and higher adsorption capacity is realized, the selectivity of pigment in caramel is enhanced, and the high-efficiency separation is realized. In order to achieve the above purpose, the technical scheme of the invention is as follows:
the preparation method of the macroporous adsorption resin for caramel decoloration comprises the following steps:
preparing macroporous adsorption resin, namely adding polyvinyl alcohol into water for dissolution, adding sodium chloride, heating, adding styrene, diethylene glycol divinyl ether, divinylbenzene, an initiator and a pore-forming agent again, uniformly mixing, standing, stirring at a low speed, preparing spheres with the required particle size, gradually heating in stages, preserving heat and shaping, washing the pore-forming agent, and pumping out a mother solution to obtain the macroporous adsorption resin;
chloromethylation is carried out on macroporous adsorption resin, and chloromethylation is carried out under the action of a metal catalyst to obtain chloromethylation microspheres;
adding phenol, solvent and Lewis acid into chloromethylation microsphere, controlling the reaction temperature to be close to the boiling point of the solvent, and obtaining the adsorption resin with high specific surface area.
Specifically, the mass ratio of the styrene to the diethylene glycol divinyl ether to the divinylbenzene is 1:2:2.
specifically, the initiator is one of dibenzoyl peroxide and azobisisobutyronitrile.
Specifically, the pore-forming agent is one of toluene, gasoline and liquid wax.
Specifically, the solvent is one of dichloroethane and nitrobenzene.
Specifically, the Lewis acid is one of zinc chloride, ferric chloride, aluminum trichloride and tin tetrachloride.
Specifically, chloromethylation is carried out on the macroporous adsorption resin, chloromethyl ether is added, zinc chloride is added, sulfuric acid is added dropwise while stirring, heat preservation is carried out, chloride ions are removed by washing, and solid-liquid separation is carried out, so that chloromethylation microspheres are obtained.
Specifically, the method further comprises the step of pretreatment of macroporous adsorption resin before chloromethylation of the macroporous adsorption resin, wherein the central particle size of the wet sieve resin is controlled to be 0.7-1.0mm.
Compared with the prior art, the preparation method of the macroporous adsorption resin for caramel decoloration has the following main beneficial effects:
the prepared macroporous adsorption resin has better caramel decoloring effect than the common adsorption resin in the market, has higher decoloring rate, is renewable, has better mechanical strength and higher adsorption capacity, and enhances the selectivity and high-efficiency separability of pigment in the caramel.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, but is apparent to those skilled in the art in view of the present invention.
Example 1:
the embodiment is a preparation method of macroporous adsorption resin for caramel decolorization, comprising the following steps:
preparing macroporous adsorption resin, namely adding 0.6g of polyvinyl alcohol and 18g of sodium chloride into 600g of water, and heating to 40 ℃ to obtain a water phase; mixing 20g of monomer styrene, 40g of diethylene glycol divinyl ether and 40g of divinylbenzene, 1.1g of dibenzoyl peroxide and 100g of toluene uniformly, adding into a water phase, standing for 5-10 minutes, and stirring at a low speed to obtain balls with the required particle size; gradually heating to 60 ℃ within 30 minutes, gradually heating to 65 ℃ within 30 minutes, heating to 68 ℃ and preserving heat for shaping, heating to 75 ℃ and preserving heat for 1.5 hours, heating to 80 ℃ and preserving heat for 2 hours, heating to 90 ℃ and preserving heat for 2 hours, then cooling to 60 ℃, and draining mother liquor to obtain the macroporous adsorption resin.
Pretreating macroporous adsorption resin, stirring and washing with hot water at 60 ℃ for half an hour, rapidly stirring each time until water is discharged to be clear, pumping water washing liquid as much as possible, adding methylal to control the temperature to 20 ℃, extracting pore-forming agent toluene until water is added and no large oil bloom exists, adding water into the resin for washing, adding hydrochloric acid solution with the concentration of 5% for washing, and washing with water to be neutral; the wet sieve resin control center particle size was 0.7mm.
50g of macroporous adsorption resin microspheres obtained in the steps are taken and placed in 150 g of chloromethyl ether, 20g of anhydrous zinc chloride solution is added, 30ml of sulfuric acid is dropwise added while stirring, the reaction temperature is controlled to be 30 ℃, the temperature is kept for 10 hours, and the microspheres are washed with water to remove chloride ions; after stirring, carrying out solid-liquid separation to obtain chloromethylation microspheres.
Swelling the chloromethylated microsphere obtained in the above steps until the volume is not increased, then adding phenol accounting for 5% of the mass of the chloromethylated microsphere, adding 500ml of dichloroethane and 40g of zinc chloride, reacting under the action of Lewis acid, controlling the boiling point temperature close to that of the solvent, and reacting for 6 hours to obtain the macroporous adsorption resin with high specific surface area.
Example 2:
the embodiment is a preparation method of macroporous adsorption resin for caramel decolorization, comprising the following steps:
preparing macroporous adsorption resin, namely adding 0.6g of polyvinyl alcohol and 18g of sodium chloride into 600g of water, and heating to 40 ℃ to obtain a water phase; mixing 20g of monomer styrene, 40g of diethylene glycol divinyl ether, 40g of divinylbenzene, 1.1g of azodiisobutyronitrile and 100g of gasoline uniformly, adding the mixture into a water phase, standing for 5-10 minutes, and stirring at a low speed to obtain balls with the required particle size; gradually heating to 60 ℃ within 30 minutes, gradually heating to 65 ℃ within 30 minutes, heating to 68 ℃ and preserving heat for shaping, heating to 75 ℃ and preserving heat for 1.5 hours, heating to 80 ℃ and preserving heat for 2 hours, heating to 90 ℃ and preserving heat for 2 hours, then cooling to 50 ℃, draining mother liquor, and obtaining the macroporous adsorption resin.
Pretreating macroporous adsorption resin, stirring and washing with hot water at 50 ℃ for half an hour, rapidly stirring each time until water is discharged to be clear, pumping water washing liquid as much as possible, adding methylal to control the temperature to 20 ℃, extracting pore-forming agent gasoline until water is added and no large oil is left, adding water into the resin for washing, adding hydrochloric acid solution with the concentration of 5% for washing, and washing with water to be neutral; the wet sieve resin control center particle size was 1.0mm.
50g of macroporous adsorption resin microspheres obtained in the steps are taken and placed in 150 g of chloromethyl ether, 20g of anhydrous zinc chloride solution is added, 30ml of sulfuric acid is dropwise added while stirring, the reaction temperature is controlled to be 30 ℃, the temperature is kept for 10 hours, and the microspheres are washed with water to remove chloride ions; after stirring, carrying out solid-liquid separation to obtain chloromethylation microspheres.
Swelling the chloromethylated microsphere obtained in the above steps until the volume is not increased, then adding phenol accounting for 5% of the mass of the chloromethylated microsphere, adding 500ml of nitrobenzene and 40g of ferric trichloride, reacting under the action of Lewis acid, controlling the boiling point temperature close to that of the solvent, and obtaining the macroporous adsorption resin with high specific surface area for 6 hours.
Example 3:
the embodiment is a preparation method of macroporous adsorption resin for caramel decolorization, comprising the following steps:
preparing macroporous adsorption resin, namely adding 0.6g of polyvinyl alcohol and 18g of sodium chloride into 600g of water, and heating to 40 ℃ to obtain a water phase; mixing 20g of monomer styrene, 40g of diethylene glycol divinyl ether and 40g of divinylbenzene, 1.1g of azodiisobutyronitrile and 100g of liquid wax, adding into a water phase after fully mixing, standing for 5-10 minutes, and stirring at a low speed to obtain balls with the required particle size; gradually heating to 60 ℃ within 30 minutes, gradually heating to 65 ℃ within 30 minutes, heating to 68 ℃ and preserving heat for shaping, heating to 75 ℃ and preserving heat for 1.5 hours, heating to 80 ℃ and preserving heat for 2 hours, heating to 90 ℃ and preserving heat for 2 hours, then cooling to 50 ℃, draining mother liquor, and obtaining the macroporous adsorption resin.
Pretreating macroporous adsorption resin, stirring and washing with 50 ℃ hot water, stirring rapidly for half an hour each time until water is discharged to be clear, pumping water washing liquid as much as possible, adding methylal to control the temperature to 20 ℃, extracting Kong Jiye wax until water is added and no large oil bloom exists, adding water into the resin for washing, adding 5% hydrochloric acid solution for washing, and washing with water to be neutral; the wet sieve resin controlled the center particle size to be 0.8mm.
50g of macroporous adsorption resin microspheres obtained in the steps are taken and placed in 150 g of chloromethyl ether, 20g of anhydrous zinc chloride solution is added, 30ml of sulfuric acid is dropwise added while stirring, the reaction temperature is controlled to be 30 ℃, the temperature is kept for 10 hours, and the microspheres are washed with water to remove chloride ions; after stirring, carrying out solid-liquid separation to obtain chloromethylation microspheres.
Swelling the chloromethylated microsphere obtained in the above steps until the volume is not increased, then adding phenol accounting for 7% of the mass of the chloromethylated microsphere, adding 500ml of nitrobenzene and 40g of aluminum trichloride, reacting under the action of Lewis acid, controlling the boiling point temperature close to that of the solvent, and obtaining the macroporous adsorption resin with high specific surface area for 6 hours.
Example 4:
the embodiment is a preparation method of macroporous adsorption resin for caramel decolorization, comprising the following steps:
preparing macroporous adsorption resin, namely adding 0.6g of polyvinyl alcohol and 18g of sodium chloride into 600g of water, and heating to 40 ℃ to obtain a water phase; mixing 20g of monomer styrene, 40g of diethylene glycol divinyl ether and 40g of divinylbenzene, 1.1g of azodiisobutyronitrile and 100g of liquid wax, adding into a water phase after fully mixing, standing for 5-10 minutes, and stirring at a low speed to obtain balls with the required particle size; gradually heating to 60 ℃ within 30 minutes, gradually heating to 65 ℃ within 30 minutes, heating to 68 ℃ and preserving heat for shaping, heating to 75 ℃ and preserving heat for 1.5 hours, heating to 80 ℃ and preserving heat for 2 hours, heating to 90 ℃ and preserving heat for 2 hours, then cooling to 50 ℃, draining mother liquor, and obtaining the macroporous adsorption resin.
Pretreating macroporous adsorption resin, stirring and washing with 50 ℃ hot water, stirring rapidly for half an hour each time until water is discharged to be clear, pumping water washing liquid as much as possible, adding methylal to control the temperature to 20 ℃, extracting Kong Jiye wax until water is added and no large oil bloom exists, adding water into the resin for washing, adding 5% hydrochloric acid solution for washing, and washing with water to be neutral; the wet sieve resin controlled the center particle size to be 0.8mm.
50g of macroporous adsorption resin microspheres obtained in the steps are taken and placed in 150 g of chloromethyl ether, 20g of anhydrous zinc chloride solution is added, 30ml of sulfuric acid is dropwise added while stirring, the reaction temperature is controlled to be 30 ℃, the temperature is kept for 10 hours, and the microspheres are washed with water to remove chloride ions; after stirring, carrying out solid-liquid separation to obtain chloromethylation microspheres.
Swelling the chloromethylated microsphere obtained in the above steps until the volume is not increased, then adding phenol accounting for 12% of the mass of the chloromethylated microsphere, adding 500ml of nitrobenzene and 40g of stannic chloride, reacting under the action of Lewis acid, controlling the boiling point temperature close to that of the solvent, and obtaining the macroporous adsorption resin with high specific surface area for 6 hours.
Examples 1-4 wood activated carbon test methods were performed to determine caramel discoloration rates:
as shown in the test data in the table, example 2 has a better decoloring effect than example 1, and the decoloring effect of the resin can be improved by increasing the polarity of the resin due to the fact that the solvent nitrobenzene participates in the chloromethyl reaction in a small amount. As can be seen from examples 2,3,4, the discoloration effect of the resin increases as the amount of phenol added increases, and the discoloration effect of the resin also increases as the amount of phenolic hydroxyl groups introduced by the reaction increases. However, the amount of phenol increased from 7% to 12%, and the decoloring effect of the resin increased only slightly, indicating that the decoloring effect of the resin did not change significantly by increasing the amount of added phenol after increasing the amount of phenol to a certain amount.
When the embodiment is applied, the prepared macroporous adsorption resin has better caramel decoloring effect than the common adsorption resin in the market, has higher decoloring rate, is renewable, has better mechanical strength and higher adsorption capacity, and enhances the selectivity and high-efficiency separability of pigment in the caramel.
In the description of the present specification, the terms "one embodiment," "some embodiments," "particular embodiments," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Although the embodiments of the present invention are described above, the embodiments are only used for facilitating understanding of the present invention, and are not intended to limit the present invention. Any person skilled in the art can make any modification and variation in form and detail without departing from the spirit and scope of the present disclosure, but the scope of the present disclosure is to be determined by the appended claims.
Claims (8)
1. The preparation method of the macroporous adsorption resin for caramel decoloration is characterized by comprising the following steps:
preparing macroporous adsorption resin, namely adding polyvinyl alcohol into water for dissolution, adding sodium chloride, heating, adding styrene, diethylene glycol divinyl ether, divinylbenzene, an initiator and a pore-forming agent again, uniformly mixing, standing, stirring at a low speed, preparing spheres with the required particle size, gradually heating in stages, preserving heat and shaping, washing the pore-forming agent, and pumping out a mother solution to obtain the macroporous adsorption resin;
chloromethylation is carried out on macroporous adsorption resin, and chloromethylation is carried out under the action of a metal catalyst to obtain chloromethylation microspheres;
adding phenol, solvent and Lewis acid into chloromethylation microsphere, controlling the reaction temperature to be close to the boiling point of the solvent, and obtaining the adsorption resin with high specific surface area.
2. The method for preparing macroporous adsorption resin for caramel decolorization according to claim 1, wherein: the mass ratio of the styrene to the diethylene glycol divinyl ether to the divinylbenzene is 1:2:2.
3. the method for preparing macroporous adsorption resin for caramel decolorization according to claim 1, wherein: the initiator is one of dibenzoyl peroxide and azobisisobutyronitrile.
4. The method for preparing macroporous adsorption resin for caramel decolorization according to claim 1, wherein: the pore-forming agent is one of toluene, gasoline and liquid wax.
5. The method for preparing macroporous adsorption resin for caramel decolorization according to claim 1, wherein: the solvent is one of dichloroethane and nitrobenzene.
6. The method for preparing macroporous adsorption resin for caramel decolorization according to claim 1, wherein: the Lewis acid is one of zinc chloride, ferric trichloride, aluminum trichloride and stannic tetrachloride.
7. The method for preparing macroporous adsorption resin for caramel decolorization according to claim 1, wherein: and (3) chloromethylating the macroporous adsorption resin, adding chloromethyl ether, adding zinc chloride, dropwise adding sulfuric acid while stirring, preserving heat, washing with water to remove chloride ions, and carrying out solid-liquid separation to obtain chloromethylated microspheres.
8. The method for preparing macroporous adsorption resin for caramel decolorization according to claim 1, wherein: the macroporous adsorption resin is subjected to chloromethylation, and the pretreatment of the macroporous adsorption resin is further included, wherein the particle size of the center of the wet sieve resin is controlled to be 0.7-1.0mm.
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Denomination of invention: Preparation method of macroporous adsorption resin for caramel decolorization Granted publication date: 20230718 Pledgee: Bank of Communications Co.,Ltd. Suzhou Sub branch in Jiangsu Pilot Free Trade Zone Pledgor: Jiangsu Jinshan New Material Co.,Ltd. Registration number: Y2024980005407 |
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