CN111826088B - Production process of high-water-solubility ultra-light-color rosin resin - Google Patents
Production process of high-water-solubility ultra-light-color rosin resin Download PDFInfo
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- CN111826088B CN111826088B CN202010808282.3A CN202010808282A CN111826088B CN 111826088 B CN111826088 B CN 111826088B CN 202010808282 A CN202010808282 A CN 202010808282A CN 111826088 B CN111826088 B CN 111826088B
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- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 title claims abstract description 142
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 title claims abstract description 142
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 title claims abstract description 142
- 239000011347 resin Substances 0.000 title claims abstract description 74
- 229920005989 resin Polymers 0.000 title claims abstract description 74
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 38
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 31
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 29
- CZNRFEXEPBITDS-UHFFFAOYSA-N 2,5-bis(2-methylbutan-2-yl)benzene-1,4-diol Chemical compound CCC(C)(C)C1=CC(O)=C(C(C)(C)CC)C=C1O CZNRFEXEPBITDS-UHFFFAOYSA-N 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 19
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 238000007259 addition reaction Methods 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 14
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical compound OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 claims abstract description 13
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 13
- 238000005886 esterification reaction Methods 0.000 claims abstract description 13
- 239000000194 fatty acid Substances 0.000 claims abstract description 13
- 229930195729 fatty acid Natural products 0.000 claims abstract description 13
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 13
- 239000011265 semifinished product Substances 0.000 claims abstract description 13
- 239000001530 fumaric acid Substances 0.000 claims abstract description 9
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000007599 discharging Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 23
- 238000001914 filtration Methods 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 12
- 238000010298 pulverizing process Methods 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 230000032050 esterification Effects 0.000 claims description 3
- 239000002270 dispersing agent Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052810 boron oxide Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 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
- 239000002904 solvent Substances 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- -1 welding aids Substances 0.000 description 2
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241000283986 Lepus Species 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000000025 natural resin Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; OIL DRYING AGENTS, i.e. SICCATIVES; TURPENTINE
- C09F1/00—Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
- C09F1/04—Chemical modification, e.g. esterification
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a production process of high-water-solubility ultra-light-color rosin resin, which comprises the following steps: (1) crushing rosin; (2) adding ethanol into the rosin crushed material, heating while stirring to completely dissolve rosin to prepare a rosin mixed solution; (3) adding expanded perlite powder, zirconium and 2, 5-di-tert-amyl hydroquinone into the rosin mixed solution, then adding fumaric acid, and heating to perform addition reaction to obtain a rosin mixture; (4) adding 1, 4-butanediol into the rosin mixture, adding nickel and aluminum oxide, and performing esterification reaction to obtain a rosin resin semi-finished product; (5) adding a diffusant NNO and fatty acid sorbitan into the rosin resin, preserving heat, discharging and cooling to obtain the high-water-solubility ultra-light-color rosin resin. The rosin resin produced by the invention has the advantages of high water solubility, light color, large viscosity, good stability, environmental protection, no odor, transparency and the like, and is low in production cost, environment-friendly and safe, and can be widely popularized and applied.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the technical field of deep processing of rosin resin, and particularly relates to a production process of high-water-solubility ultra-light-color rosin resin.
[ background of the invention ]
Rosin is a renewable mixed natural resin and is one of the most important products in forest chemical industry in China. At present, rosin is widely applied to industrial production as a modifier and an additive, and is widely applied to the fields of coatings, printing ink, paints, adhesives, welding aids, rubber, papermaking, food additives, biological products and the like, but because rosin has instability, such as easy crystallization, easy oxidation and color change, low softening point and the like, the performance and the application field of the rosin are limited, and therefore, the rosin is generally subjected to deep processing.
The water-soluble rosin resin is polyol rosin with light color, is prepared by using refined rosin as basic raw material and through the processes of hydrogenation, esterification, water-soluble treatment and the like, and is a novel low-pollution, energy-saving and resource-saving coating. The water-soluble treatment is to introduce hydrophilic groups or solubilizing groups into the resin to make it a coating material using water as a dissolving medium. The processing method of the existing water-soluble rosin resin mainly comprises a solvent method, a high-pressure melting method and an ultrasonic emulsification method. For the solvent method, the prepared rosin emulsion contains organic solvent harmful to human body, and has the problems of poor viscosity, opacity, high production difficulty, poor compatibility and the like. For the high-pressure melting method and the ultrasonic emulsification method, the preparation process has high requirements on equipment and operation conditions and high cost.
Chinese patent application document "a water-soluble rosin resin processing device and an application method thereof (application publication No. CN 110721641A)" discloses a preparation method of water-soluble rosin resin, which comprises the following steps: (1) introducing nitrogen from the auxiliary material feeding pipe, evacuating the air in the reaction kettle, adding the rosin into the reaction kettle from the feeding hole, adding ethanol from the auxiliary material feeding hole, opening the stirrer, introducing heat-conducting oil from the heat-conducting oil inlet in a stirring state, heating to 140-; (2) after the rosin is dissolved, introducing a catalyst consisting of metalloporphyrin and boron oxide from an auxiliary material inlet, introducing fumaric acid from the auxiliary material inlet of the reaction kettle, continuously stirring, controlling the reaction temperature to be 80-100 ℃, reacting for 60-80min, and filtering to remove the catalyst to obtain fumaric acid modified rosin; (3) pentaerythritol is added from an auxiliary material inlet, a catalyst consisting of metalloporphyrin and boron oxide is added, the reaction temperature is controlled at 180 ℃ and 220 ℃, and the esterification reaction lasts for 1-2 h; (4) under the stirring state, adding a surfactant from auxiliary materials, wherein the surfactant consists of sodium cocoamidoalkyl sulfate and isooctanol polyoxyethylene ether phosphate, preserving the temperature at 80-100 ℃ for 20-30min, cooling to room temperature, and discharging from a material outlet to obtain the water-soluble rosin resin. The rosin resin produced by the method has the advantages of high hardness, environmental protection, no odor, transparency and the like, but has the problems of low water solubility, high color and the like, and can not meet the requirements of popularization and application.
[ summary of the invention ]
The invention provides a production process of a high-water-solubility ultra-light-color rosin resin, which aims to solve the problems of low water solubility, high color and luster and the like of the existing water-soluble rosin resin.
In order to solve the technical problems, the invention adopts the following technical scheme:
a production process of a high-water-solubility ultra-light-color rosin resin comprises the following steps:
(1) pulverizing rosin to obtain pulverized rosin;
(2) taking the weight part as a unit, adding 180-300 parts of ethanol into 120 parts of the rosin crushed material prepared in the step (1), and heating under stirring to completely dissolve the rosin to prepare a rosin mixed solution;
(3) adding 2.4-3.6 parts by weight of expanded perlite powder, zirconium and 2, 5-di-tert-amyl hydroquinone into the rosin mixed solution prepared in the step (2), then adding fumaric acid accounting for 6.2-9.5% of the rosin, heating for addition reaction, and filtering to remove the expanded perlite powder and the zirconium to prepare a rosin mixture;
(4) taking parts by weight as a unit, adding 16-30 parts of 1, 4-butanediol into the rosin mixture prepared in the step (3), then adding 2.3-3.5 parts of nickel and aluminum oxide by weight for esterification, and filtering to remove nickel and aluminum oxide to prepare a rosin resin semi-finished product;
(5) and (3) after cooling, adding 6-11 parts by weight of a diffusant NNO and fatty acid sorbitan into the semi-finished product of the rosin resin prepared in the step (4) by taking parts by weight as a unit, preserving the heat for 35-50min, discharging and cooling to prepare the high-water-solubility ultra-light-color rosin resin.
Further, the mass concentration of the ethanol in the step (2) is 80-90%.
Further, the stirring speed in the step (2) is 100-200 r/min.
Further, the temperature in step (2) is raised to 165-169 ℃.
Further, the weight ratio of the expanded perlite powder, the zirconium and the 2, 5-di-tert-amyl hydroquinone in the step (3) is 5-12:23-65: 2-3.
Further, the temperature is increased in the step (3) to carry out the addition reaction: heating to 180 ℃ and 200 ℃, and carrying out addition reaction for 50-62 min.
Further, the weight ratio of the nickel to the alumina in the step (4) is 3-5: 0.8-1.4.
Further, the conditions for carrying out the esterification reaction in the step (4): the esterification reaction is carried out for 1 to 1.5 hours at the temperature of 270 ℃ and 278 ℃.
Further, the weight ratio of the dispersing agent NNO to the fatty acid sorbitan in the step (5) is 8-13: 15-24.
Further, the temperature of the heat preservation in the step (5) is 106-.
The invention has the following beneficial effects:
(1) the water-solubility, the color and the viscosity of the water-soluble rosin resin prepared by the method are obviously higher, lighter and larger than those of the water-soluble rosin resin prepared by the prior art, and the water-soluble rosin resin is at least 24 times higher, at least 10 hasen color numbers lighter and at least 396mPa.s larger.
(2) In the preparation process, the expanded perlite powder, the zirconium and the 2, 5-di-tert-amyl hydroquinone play a synergistic role in the addition reaction, and the color of the water-soluble rosin resin is obviously reduced; the zirconium plays a role in catalysis, the expanded perlite powder can disperse the zirconium, so that the effective area is increased, the activity of the expanded perlite powder is obviously improved, the strength of the zirconium catalysis is increased, and in addition, the 2, 5-di-tert-amyl hydroquinone can play a role in lightening and stabilizing the color of the resin, so that the color of the water-soluble rosin resin is obviously reduced under the coordination and synergism of the expanded perlite powder, the zirconium and the 2, 5-di-tert-amyl hydroquinone in the addition reaction.
(3) The rosin resin produced by the invention has the advantages of high viscosity, good stability, environmental protection, no odor, transparency and the like, and has excellent indexes.
(4) The preparation process has the advantages of low production cost, environmental protection, safety, easy realization of industrial production and the like, and can be widely popularized and applied.
[ description of the drawings ]
FIG. 1 is a flow chart of the preparation process of the high water-solubility ultra-light color rosin resin of the invention.
[ detailed description ] embodiments
In order to facilitate a better understanding of the invention, the following examples are given to illustrate, but not to limit the scope of the invention.
In an embodiment, the production process of the high water-solubility ultra-light-colored rosin resin comprises the following steps:
(1) pulverizing rosin to obtain pulverized rosin;
(2) taking the weight part as a unit, adding 180-300 parts of ethanol with the mass concentration of 80-90% into 120 parts of the rosin crushed material prepared in the step (1), heating to 165-169 ℃ at the rotating speed of 100-200r/min, and completely dissolving the rosin to prepare a rosin mixed solution;
(3) adding 2.4-3.6 parts by weight of expanded perlite powder, zirconium and 2, 5-di-tert-amyl hydroquinone into the rosin mixed solution prepared in the step (2) by taking parts by weight as units, wherein the weight ratio of the expanded perlite powder to the zirconium to the 2, 5-di-tert-amyl hydroquinone is 5-12:23-65:2-3, adding fumaric acid accounting for 6.2-9.5% of the weight of the rosin, heating to 180-200 ℃, carrying out addition reaction for 50-62min, and filtering to remove the expanded perlite powder and the zirconium to prepare a rosin mixture;
(4) adding 16-30 parts of 1, 4-butanediol, then adding 2.3-3.5 parts of nickel and alumina by weight, wherein the weight ratio of the nickel to the alumina is 3-5:0.8-1.4, carrying out esterification reaction at the temperature of 270-278 ℃ for 1-1.5h, and filtering to remove the nickel and the alumina to obtain a rosin resin semi-finished product;
(5) and (3) after cooling, adding 6-11 parts by weight of a diffusant NNO and fatty acid sorbitan to the semi-finished product of the rosin resin prepared in the step (4) by taking parts by weight as a unit, wherein the weight ratio of the diffusant NNO to the fatty acid sorbitan is 8-13:15-24, preserving heat for 35-50min at the temperature of 106-125 ℃, discharging and cooling to prepare the high-water-solubility ultra-light-color rosin resin.
The present invention is illustrated by the following more specific examples.
Example 1
A production process of a high-water-solubility ultra-light-color rosin resin comprises the following steps:
(1) pulverizing rosin to obtain pulverized rosin;
(2) adding 250 parts by weight of 86% ethanol into 114 parts by weight of the rosin crushed material prepared in the step (1), and heating to 168 ℃ at a rotation speed of 200r/min to completely dissolve rosin to prepare a rosin mixed solution;
(3) adding 3 parts by weight of expanded perlite powder, zirconium and 2, 5-di-tert-amyl hydroquinone into the rosin mixed solution prepared in the step (2) by taking parts by weight as units, wherein the weight ratio of the expanded perlite powder to the zirconium to the 2, 5-di-tert-amyl hydroquinone is 10:43:2, adding fumaric acid accounting for 8.6% of the weight of the rosin, heating to 190 ℃, carrying out addition reaction for 55min, and filtering to remove the expanded perlite powder and the zirconium to prepare a rosin mixture;
(4) adding 25 parts of 1, 4-butanediol into the rosin mixture prepared in the step (3) by weight, adding 3 parts of nickel and aluminum oxide by weight, wherein the weight ratio of the nickel to the aluminum oxide is 4:1.2, performing esterification reaction at 275 ℃ for 1.3h, and filtering to remove the nickel and the aluminum oxide to prepare a rosin resin semi-finished product;
(5) and (3) after cooling, adding 10 parts by weight of a diffusant NNO and a fatty acid sorbitan into the semi-finished product of the rosin resin prepared in the step (4) by taking parts by weight as a unit, keeping the temperature at 118 ℃ for 42min, discharging and cooling to prepare the high-water-solubility ultra-light-color rosin resin, wherein the weight ratio of the diffusant NNO to the fatty acid sorbitan is 10: 19.
Example 2
A production process of a high-water-solubility ultra-light-color rosin resin comprises the following steps:
(1) pulverizing rosin to obtain pulverized rosin;
(2) adding 200 parts by weight of 82% ethanol into 108 parts by weight of the rosin crushed material prepared in the step (1), and heating to 165 ℃ at a rotation speed of 100r/min to completely dissolve rosin to prepare a rosin mixed solution;
(3) adding 2.5 parts by weight of expanded perlite powder, zirconium and 2, 5-di-tert-amyl hydroquinone into the rosin mixed solution prepared in the step (2) by taking parts by weight as units, wherein the weight ratio of the expanded perlite powder to the zirconium to the 2, 5-di-tert-amyl hydroquinone is 6:25:2, adding fumaric acid accounting for 6.5 percent of the weight of the rosin, heating to 180 ℃, carrying out addition reaction for 60min, and filtering to remove the expanded perlite powder and the zirconium to prepare a rosin mixture;
(4) taking parts by weight as a unit, adding 17 parts of 1, 4-butanediol into the rosin mixture prepared in the step (3), adding 2.6 parts of nickel and aluminum oxide by weight, wherein the weight ratio of the nickel to the aluminum oxide is 3:0.9, carrying out esterification reaction at the temperature of 270 ℃ for 1.5h, and filtering to remove the nickel and the aluminum oxide to prepare a rosin resin semi-finished product;
(5) and (3) after cooling, adding 6 parts by weight of a diffusant NNO and fatty acid sorbitan to the semi-finished product of the rosin resin prepared in the step (4) by taking parts by weight as a unit, wherein the weight ratio of the diffusant NNO to the fatty acid sorbitan is 8:17, keeping the temperature at 108 ℃ for 48min, discharging and cooling to prepare the high-water-solubility ultra-light-color rosin resin.
Example 3
A production process of a high-water-solubility ultra-light-color rosin resin comprises the following steps:
(1) pulverizing rosin to obtain pulverized rosin;
(2) taking parts by weight as a unit, adding 280 parts of 88 mass percent ethanol into 118 parts of the rosin crushed material prepared in the step (1), heating to 167 ℃ at a rotating speed of 200r/min, and completely dissolving rosin to prepare a rosin mixed solution;
(3) adding 3.5 parts by weight of expanded perlite powder, zirconium and 2, 5-di-tert-amyl hydroquinone into the rosin mixed solution prepared in the step (2) by taking parts by weight as units, wherein the weight ratio of the expanded perlite powder to the zirconium to the 2, 5-di-tert-amyl hydroquinone is 11:63:3, adding fumaric acid accounting for 9% of the weight of the rosin, heating to 200 ℃, carrying out addition reaction for 50min, and filtering to remove the expanded perlite powder and the zirconium to prepare a rosin mixture;
(4) adding 28 parts of 1, 4-butanediol into the rosin mixture prepared in the step (3) by weight, adding 3.3 parts of nickel and aluminum oxide by weight, wherein the weight ratio of the nickel to the aluminum oxide is 5:1.3, performing esterification reaction 1 at 278 ℃, and filtering to remove the nickel and the aluminum oxide to prepare a rosin resin semi-finished product;
(5) and (3) after cooling, adding 10 parts by weight of a diffusant NNO and a fatty acid sorbitan into the semi-finished product of the rosin resin prepared in the step (4) by taking parts by weight as a unit, keeping the temperature at 124 ℃ for 36min, discharging and cooling to prepare the high-water-solubility ultra-light-color rosin resin, wherein the weight ratio of the diffusant NNO to the fatty acid sorbitan is 13: 22.
Comparative example 1
The process for the preparation of rosin resin of example 1 was followed except that expanded perlite powder, zirconium, 2, 5-di-tert-amylhydroquinone were absent in step (2).
Comparative example 2
The process for the preparation of rosin resin of example 1 was essentially the same except that expanded perlite powder was absent in step (2).
Comparative example 3
The process for preparing rosin resin of example 1 was substantially the same except that zirconium was absent in step (2).
Comparative example 4
The procedure used to prepare the rosin resin of example 1 was essentially the same except that 2, 5-di-tert-amylhydroquinone was absent in step (2).
Comparative example 5
The rosin resin was prepared by the process of example 1-2 using the Chinese patent application document "a water-soluble rosin resin processing apparatus and its application method (application publication No. CN 110721641A)".
The performance indexes of the rosin resins of examples 1 to 3 and comparative examples 1 to 5 were examined, and each performance index was measured in parallel three times. The test method of the water solubility of the rosin resin is as follows: a10 g water-soluble rosin resin sample was weighed in an Erlenmeyer flask, and water was added thereto, and the mixture was shaken and mixed until fine insoluble matter appeared in the mixture or insoluble matter adhered to the inner wall of the Erlenmeyer flask, and the amount of water added was read. The measurements were performed in triplicate and averaged. The water solubility was calculated as: water solubility times (mass (g) of added water)/mass (g) of rosin resin. The color was detected by the hansen colorimetry. The viscosity is measured with an SNB-2-J digital rotational viscometer, wherein the rotor specification: rotor # 27, rotation speed: 50 r/min. The results of the performance index measurements are shown in the following table.
From the above table, it can be seen that: (1) as can be seen from the water solubility (multiple times), color (Harson color number) and viscosity data measured in examples 1-3 and comparative example 5, the water solubility, color and viscosity of the water-soluble rosin resin prepared by the invention are obviously higher, obviously lighter and obviously larger than those of the water-soluble rosin resin prepared by the prior art, at least 24 times higher, at least 10 Harson color numbers lighter and at least 396mPa.s larger; in addition, as can be seen from the data obtained in examples 1 to 3, example 1 is the most preferred example.
(2) As can be seen from the color (Hassen color number) data measured in example 1 and comparative examples 1 to 4, the expanded perlite powder, the zirconium and the 2, 5-di-tert-amyl hydroquinone play a synergistic role in the addition reaction, and the color of the water-soluble rosin resin is obviously reduced; the zirconium plays a role in catalysis, the expanded perlite powder can disperse the zirconium, so that the effective area is increased, the activity of the expanded perlite powder is obviously improved, the strength of the zirconium catalysis is increased, and in addition, the 2, 5-di-tert-amyl hydroquinone can play a role in lightening and stabilizing the color of the resin, so that the color of the water-soluble rosin resin is obviously reduced under the coordination and synergism of the expanded perlite powder, the zirconium and the 2, 5-di-tert-amyl hydroquinone in the addition reaction. 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 production process of a high-water-solubility ultra-light-color rosin resin is characterized by comprising the following steps:
(1) pulverizing rosin to obtain pulverized rosin;
(2) taking the weight part as a unit, adding 180-300 parts of ethanol into 120 parts of the rosin crushed material prepared in the step (1), and heating under stirring to completely dissolve the rosin to prepare a rosin mixed solution;
(3) adding 2.4-3.6 parts by weight of expanded perlite powder, zirconium and 2, 5-di-tert-amyl hydroquinone into the rosin mixed solution prepared in the step (2), then adding fumaric acid accounting for 6.2-9.5% of the rosin, heating for addition reaction, and filtering to remove the expanded perlite powder and the zirconium to prepare a rosin mixture;
(4) taking parts by weight as a unit, adding 16-30 parts of 1, 4-butanediol into the rosin mixture prepared in the step (3), then adding 2.3-3.5 parts of nickel and aluminum oxide by weight for esterification, and filtering to remove nickel and aluminum oxide to prepare a rosin resin semi-finished product;
(5) and (3) after cooling, adding 6-11 parts by weight of a diffusant NNO and fatty acid sorbitan into the semi-finished product of the rosin resin prepared in the step (4) by taking parts by weight as a unit, preserving the heat for 35-50min, discharging and cooling to prepare the high-water-solubility ultra-light-color rosin resin.
2. The process for producing a high water-solubility pale rosin resin according to claim 1, wherein the mass concentration of ethanol in step (2) is 80 to 90%.
3. The process for producing a rosin resin with a high water solubility and a super light color as claimed in claim 1, wherein the stirring speed in the step (2) is 100-200 r/min.
4. The process for producing a rosin resin with a high water solubility and a super light color as claimed in claim 1, wherein the temperature in the step (2) is raised to 165-169 ℃.
5. The process for producing a high water-solubility ultra-light rosin resin according to claim 1, wherein the weight ratio of the expanded perlite powder, the zirconium and the 2, 5-di-tert-amyl hydroquinone in the step (3) is 5-12:23-65: 2-3.
6. The process for producing a highly water-soluble, ultra-light rosin resin according to claim 1, wherein the addition reaction is carried out at elevated temperature in step (3): heating to 180 ℃ and 200 ℃, and carrying out addition reaction for 50-62 min.
7. The process for producing a high water-solubility pale rosin resin according to claim 1, wherein the weight ratio of nickel to alumina in step (4) is 3-5: 0.8-1.4.
8. The process for producing a highly water-soluble, ultra-light rosin resin according to claim 1, wherein the esterification reaction in step (4) is carried out under the following conditions: the esterification reaction is carried out for 1 to 1.5 hours at the temperature of 270 ℃ and 278 ℃.
9. The production process of the high water-solubility ultra-light rosin resin as claimed in claim 1, wherein the weight ratio of the dispersant NNO to the fatty acid sorbitan in step (5) is 8-13: 15-24.
10. The process for producing a rosin resin with a high water solubility and a super light color as claimed in claim 1, wherein the temperature for the heat preservation in the step (5) is 106-125 ℃.
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