CN106905854B - Preparation method of rosin pentaerythritol ester - Google Patents
Preparation method of rosin pentaerythritol ester Download PDFInfo
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- CN106905854B CN106905854B CN201710103647.0A CN201710103647A CN106905854B CN 106905854 B CN106905854 B CN 106905854B CN 201710103647 A CN201710103647 A CN 201710103647A CN 106905854 B CN106905854 B CN 106905854B
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- rosin
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- pentaerythritol
- pentaerythritol ester
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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 78
- 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 78
- 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 78
- -1 pentaerythritol ester Chemical class 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 89
- 239000003054 catalyst Substances 0.000 claims abstract description 37
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims abstract description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 229910052757 nitrogen Inorganic materials 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 22
- WHMDKBIGKVEYHS-IYEMJOQQSA-L Zinc gluconate Chemical compound [Zn+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O WHMDKBIGKVEYHS-IYEMJOQQSA-L 0.000 claims description 3
- CANRESZKMUPMAE-UHFFFAOYSA-L Zinc lactate Chemical compound [Zn+2].CC(O)C([O-])=O.CC(O)C([O-])=O CANRESZKMUPMAE-UHFFFAOYSA-L 0.000 claims description 3
- 239000011670 zinc gluconate Substances 0.000 claims description 3
- 235000011478 zinc gluconate Nutrition 0.000 claims description 3
- 229960000306 zinc gluconate Drugs 0.000 claims description 3
- 239000011576 zinc lactate Substances 0.000 claims description 3
- 229940050168 zinc lactate Drugs 0.000 claims description 3
- 235000000193 zinc lactate Nutrition 0.000 claims description 3
- CZNVSLGYWMSMKE-OPDGVEILSA-K Ferric gluconate Chemical compound [Fe+3].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O CZNVSLGYWMSMKE-OPDGVEILSA-K 0.000 claims description 2
- 150000007942 carboxylates Chemical class 0.000 abstract description 7
- 230000035484 reaction time Effects 0.000 abstract description 4
- 239000012752 auxiliary agent Substances 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 239000002253 acid Substances 0.000 description 22
- 239000002932 luster Substances 0.000 description 20
- 239000011734 sodium Substances 0.000 description 19
- 238000000034 method Methods 0.000 description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005886 esterification reaction Methods 0.000 description 4
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 description 4
- 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 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 239000004327 boric acid Substances 0.000 description 3
- 238000004737 colorimetric analysis Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- YNVZDODIHZTHOZ-UHFFFAOYSA-K 2-hydroxypropanoate;iron(3+) Chemical compound [Fe+3].CC(O)C([O-])=O.CC(O)C([O-])=O.CC(O)C([O-])=O YNVZDODIHZTHOZ-UHFFFAOYSA-K 0.000 description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 2
- VEPSWGHMGZQCIN-UHFFFAOYSA-H ferric oxalate Chemical compound [Fe+3].[Fe+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O VEPSWGHMGZQCIN-UHFFFAOYSA-H 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- NPFOYSMITVOQOS-UHFFFAOYSA-K iron(III) citrate Chemical compound [Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NPFOYSMITVOQOS-UHFFFAOYSA-K 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- WSFQLUVWDKCYSW-UHFFFAOYSA-M sodium;2-hydroxy-3-morpholin-4-ylpropane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC(O)CN1CCOCC1 WSFQLUVWDKCYSW-UHFFFAOYSA-M 0.000 description 2
- WGIWBXUNRXCYRA-UHFFFAOYSA-H trizinc;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O WGIWBXUNRXCYRA-UHFFFAOYSA-H 0.000 description 2
- 239000004246 zinc acetate Substances 0.000 description 2
- 239000011746 zinc citrate Substances 0.000 description 2
- 235000006076 zinc citrate Nutrition 0.000 description 2
- 229940068475 zinc citrate Drugs 0.000 description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 2
- WDHVIZKSFZNHJB-UHFFFAOYSA-L zinc;butanoate Chemical compound [Zn+2].CCCC([O-])=O.CCCC([O-])=O WDHVIZKSFZNHJB-UHFFFAOYSA-L 0.000 description 2
- ZPEJZWGMHAKWNL-UHFFFAOYSA-L zinc;oxalate Chemical compound [Zn+2].[O-]C(=O)C([O-])=O ZPEJZWGMHAKWNL-UHFFFAOYSA-L 0.000 description 2
- XDWXRAYGALQIFG-UHFFFAOYSA-L zinc;propanoate Chemical compound [Zn+2].CCC([O-])=O.CCC([O-])=O XDWXRAYGALQIFG-UHFFFAOYSA-L 0.000 description 2
- 239000004831 Hot glue Substances 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 229960002413 ferric citrate Drugs 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- FRVCGRDGKAINSV-UHFFFAOYSA-L iron(2+);octadecanoate Chemical compound [Fe+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O FRVCGRDGKAINSV-UHFFFAOYSA-L 0.000 description 1
- XHQSLVIGPHXVAK-UHFFFAOYSA-K iron(3+);octadecanoate Chemical compound [Fe+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XHQSLVIGPHXVAK-UHFFFAOYSA-K 0.000 description 1
- VRIVJOXICYMTAG-IYEMJOQQSA-L iron(ii) gluconate Chemical compound [Fe+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O VRIVJOXICYMTAG-IYEMJOQQSA-L 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Catalysts (AREA)
Abstract
A preparation method of rosin pentaerythritol ester is characterized in that carboxylate is used as a catalyst, and the rosin pentaerythritol ester is prepared by reacting for 1-12 hours at a mass ratio of rosin to catalyst of 50: 1-1000: 1, a mass ratio of rosin to pentaerythritol of 4: 1-8: 1, an absolute pressure of a reaction system of 10-50 kPa and a reaction temperature of 150-300 ℃. Compared with the prior art: 1. the catalyst has high catalytic activity; 2. the reaction requires low temperature and short reaction time; 3. no other auxiliary agent is needed in the reaction process.
Description
Technical Field
The invention relates to a preparation method of rosin pentaerythritol ester, in particular to a novel method for preparing rosin pentaerythritol ester by catalyzing esterification reaction of rosin and pentaerythritol through carboxylate.
Background
The rosin pentaerythritol ester has the characteristics of large molecular weight, low acid value, high hardness and softening point and the like, has better oxidation resistance, water resistance, alkali resistance and excellent stability compared with rosin glyceride, and is widely used as a tackifier for pressure-sensitive adhesives, hot melt adhesives and the like and a modifier for rubber and plastics and the like. At present, zinc oxide or boric acid is mostly adopted in the industry as a catalyst to catalyze the esterification reaction of rosin and pentaerythritol. The process has the problems of high reaction temperature, long reaction time, dark product color and the like. In addition, in order to reduce the color of the product and improve the oxidation resistance of the rosin pentaerythritol ester, auxiliaries such as a heat stabilizer, an antioxidant, a light stabilizer, an ultraviolet absorber and the like are often added in the preparation process of the rosin pentaerythritol ester. Aiming at the problems, the invention discovers that partial carboxylate has excellent catalytic performance on catalyzing rosin and pentaerythritol esterification to prepare rosin pentaerythritol ester, can realize short-time efficient synthesis of esterification reaction at lower reaction temperature, and the obtained product has light color without adding various auxiliary agents.
Disclosure of Invention
The invention aims to replace the traditional production process for preparing rosin pentaerythritol ester by catalyzing rosin and pentaerythritol with a catalyst, and develop a novel method for synthesizing the rosin pentaerythritol ester at low temperature and short time under the catalysis of the cheap, easily-obtained and efficient catalyst by using the rosin and pentaerythritol.
Based on the above, the invention relates to a preparation method of rosin pentaerythritol ester, namely a novel method for preparing rosin pentaerythritol ester by catalyzing rosin and pentaerythritol with a carboxylate catalyst. The method is characterized in that carboxylate is used as a catalyst, and the rosin pentaerythritol ester is prepared by reacting rosin and the catalyst at a mass ratio of 50: 1-1000: 1, a mass ratio of 4: 1-8: 1, an absolute pressure of a reaction system of 10-50 kPa and a reaction temperature of 150-300 ℃ for 1-12 hours; the carboxylate catalyst is one of zinc acetate, zinc propionate, zinc butyrate, zinc stearate, zinc citrate, zinc naphthenate, zinc oxalate, zinc lactate, zinc gluconate, iron acetate, iron stearate, iron citrate, iron naphthenate, iron oxalate, iron lactate or iron gluconate.
The method is characterized in that the reaction conditions are that the mass ratio of rosin to carboxylate catalyst is 100: 1-500: 1, the mass ratio of rosin to pentaerythritol is 5: 1-6: 1, the reaction temperature is 180-270 ℃, the absolute pressure of the reaction system is 15-40 kPa, and the reaction time is 6-10 h.
The invention solves the technical problem by the following technical scheme:
the specific technical scheme is illustrated by taking an iron acetate catalyst as an example.
Putting 100.0g of rosin, 1.0g of catalyst iron acetate and 20.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 30kPa, heating to 230 ℃, stirring and reacting for 6 hours to obtain a product, namely rosin pentaerythritol ester, wherein the yield of the product is 92.3%, the acid value is 20.3mgKOH/g, the colorimetric softening point is 96.4 ℃, and the color and luster are 3 measured by adding Na, and the yield of the rosin pentaerythritol ester is the ratio of the quality of the obtained product to the total quality of the rosin and the pentaerythritol.
Compared with the traditional preparation method, the invention is characterized in that:
1. the catalyst has high catalytic activity.
2. The reaction requires low temperature and short reaction time.
3. No other auxiliary agent is needed in the reaction process.
Detailed description of the invention
The process of the present invention is further illustrated by the following examples, which are not intended to be limiting.
Example 1: putting 100.0g of rosin, 1.0g of catalyst iron acetate and 20.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 30kPa, heating to 230 ℃, stirring and reacting for 6 hours to obtain a product, namely rosin pentaerythritol ester, wherein the yield is 92.3%, the acid value is 20.3mgKOH/g, the colorimetric softening point is 96.4 ℃, and the color and luster are 3 measured by adding Na.
Comparative example 1: putting 100.0g of rosin, 1.0g of catalyst zinc oxide and 20.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 30kPa, heating to 230 ℃, stirring and reacting for 6 hours to obtain a product, namely rosin pentaerythritol ester, wherein the yield is 96.5%, the acid value is 39.6mgKOH/g, the colorimetric softening point is 97.0 ℃, and the color and luster are 7 measured by adding Na.
Comparative example 2: putting 100.0g of rosin, 1.0g of boric acid catalyst and 20.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 30kPa, heating to 230 ℃, stirring and reacting for 6 hours to obtain a product, namely rosin pentaerythritol ester, wherein the yield is 95.0%, the acid value is 42.0mgKOH/g, the softening point is 106.4 ℃, and the color and luster are measured by Ganna colorimetry to be 8.
Comparative example 3: putting 100.0g of rosin, 1.0g of catalyst zinc oxide and 20.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer and an oil-water separator, replacing air in a reaction system with 200kPa nitrogen for 5 times, heating to 270 ℃, stirring and reacting for 10 hours to obtain a product, namely rosin pentaerythritol ester, wherein the yield is 97.4%, the acid value is 26.3mgKOH/g, the softening point is 102.3 ℃, and the color is 9 according to sodium colorimetry.
Comparative example 4: 100.0g of rosin, 1.0g of boric acid catalyst and 20.0g of pentaerythritol are put into a reaction kettle provided with a stirrer, a thermometer and an oil-water separator, air in a reaction system is replaced by 200kPa nitrogen for 5 times, the reaction system is heated to 270 ℃, and after stirring reaction is carried out for 10 hours, the product rosin pentaerythritol ester is obtained, wherein the yield is 97.8 percent, the acid value is 28.6mgKOH/g, the softening point is 98.3 ℃, and the color and luster are 10 measured by sodium colorimetry.
Example 2: putting 100.0g of rosin, 1.0g of catalyst iron naphthenate and 20.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 20kPa, heating to 230 ℃, stirring and reacting for 8 hours to obtain a product, namely rosin pentaerythritol ester, wherein the yield is 95.0%, the acid value is 23.8mgKOH/g, the colorimetric softening point is 95.6 ℃, and the color and luster are 5 measured by adding Na.
Example 3: putting 100.0g of rosin, 2.0g of catalyst zinc acetate and 15.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 20kPa, heating to 280 ℃, stirring and reacting for 4 hours to obtain a product, namely rosin pentaerythritol ester, wherein the yield is 95.0%, the acid value is 18.9mgKOH/g, the colorimetric softening point is 98.2 ℃, and the color and luster are 3 measured by adding Na.
Example 4: putting 100.0g of rosin, 1.8g of zinc propionate catalyst and 13.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 10kPa, heating to 250 ℃, stirring and reacting for 6 hours to obtain a product, namely rosin pentaerythritol ester, wherein the yield is 93.0%, the acid value is 22.3g KOH/g, the colorimetric softening point is 96.3 ℃, and the color and luster are 3 measured by adding Na.
Example 5: putting 100.0g of rosin, 1.5g of zinc butyrate serving as a catalyst and 14.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 20kPa, heating to 240 ℃, and stirring for reaction for 7 hours to obtain a product, namely rosin pentaerythritol ester, wherein the yield is 94.2%, the acid value is 22.0mgKOH/g, the colorimetric softening point is 98.6 ℃, and the color and luster are 3 measured by adding Na.
Example 6: putting 100.0g of rosin, 2.0g of catalyst zinc stearate and 18.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 20kPa, heating to 240 ℃, stirring and reacting for 9 hours to obtain a product, namely rosin pentaerythritol ester, wherein the yield is 95.6%, the acid value is 21.9mgKOH/g, the colorimetric softening point is 96.8 ℃, and the color and luster are 4 measured by adding Na.
Example 7: putting 100.0g of rosin, 2.0g of catalyst zinc citrate and 15.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 40kPa, heating to 250 ℃, stirring and reacting for 8 hours to obtain a product, namely rosin pentaerythritol ester, wherein the yield is 95.3%, the acid value is 22.6mgKOH/g, the colorimetric softening point is 94.5 ℃, and the color and luster are 4 measured by adding Na.
Example 8: putting 100.0g of rosin, 2.0g of catalyst zinc naphthenate and 20.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 40kPa, heating to 260 ℃, stirring and reacting for 3 hours to obtain a product, namely rosin pentaerythritol ester, wherein the yield is 95.1%, the acid value is 24.2mgKOH/g, the colorimetric softening point is 98.6 ℃, and the color and luster are 4 measured by adding Na.
Example 9: putting 100.0g of rosin, 2.2g of zinc oxalate as a catalyst and 13.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 20kPa, heating to 270 ℃, stirring and reacting for 8 hours to obtain a product, namely the rosin pentaerythritol ester, wherein the yield is 96.2%, the acid value is 21.9mgKOH/g, the colorimetric softening point is 98.0 ℃, and the color and luster are 4 measured by adding Na.
Example 10: putting 100.0g of rosin, 1.5g of catalyst zinc lactate and 20.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 40kPa, heating to 200 ℃, stirring and reacting for 7 hours to obtain a product, namely rosin pentaerythritol ester, wherein the yield is 94.4%, the acid value is 24.3mgKOH/g, the colorimetric softening point is 95.5 ℃, and the color and luster are 3 measured by adding Na.
Example 11: 100.0g of rosin, 0.50g of zinc gluconate serving as a catalyst and 22.0g of pentaerythritol are put into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, the air in a reaction system is replaced by nitrogen with 200kPa for 5 times, the vacuum system is started, the absolute pressure of the reaction system is controlled to be 10kPa, the reaction system is heated to 180 ℃, the reaction is stirred for 8 hours, the product rosin pentaerythritol ester is obtained, and the yield is 95.6%, the acid value is 23.0mgKOH/g, the softening point is 97.2 ℃, and the color and luster are 3 measured by color comparison with sodium.
Example 12: putting 100.0g of rosin, 1.8g of catalyst ferric stearate and 19.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 15kPa, heating to 250 ℃, stirring and reacting for 4 hours to obtain a product, namely rosin pentaerythritol ester, wherein the yield is 95.0%, the acid value is 24.6mgKOH/g, the colorimetric softening point is 93.4 ℃, and the color and luster are 4 measured by adding Na.
Example 13: putting 100.0g of rosin, 1.0g of ferric citrate as a catalyst and 18.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 40kPa, heating to 250 ℃, stirring and reacting for 4 hours to obtain a product, namely the rosin pentaerythritol ester, wherein the yield is 94.6%, the acid value is 23.6mgKOH/g, the colorimetric softening point is 98.0 ℃, and the color and luster are 4 as measured by adding Na.
Example 14: putting 100.0g of rosin, 1.5g of catalyst iron oxalate and 15.0g of pentaerythritol into a reaction kettle equipped with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 40kPa, heating to 270 ℃, stirring and reacting for 4 hours to obtain a product, namely rosin pentaerythritol ester, wherein the yield is 95.5%, the acid value is 23.8mgKOH/g, the colorimetric softening point is 94.6 ℃, and the color and luster are 3 measured by adding Na.
Example 15: putting 100.0g of rosin, 2.0g of catalyst iron lactate and 12.5g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 50kPa, heating to 300 ℃, stirring and reacting for 1h to obtain a product, namely rosin pentaerythritol ester, wherein the yield is 97.3%, the acid value is 29.8mgKOH/g, the colorimetric softening point is 96.8 ℃, and the color and luster are 5 measured by adding Na.
Example 16: putting 100.0g of rosin, 0.1g of catalyst ferric gluconate and 25.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 10kPa, heating to 150 ℃, stirring and reacting for 12 hours to obtain a product, namely the rosin pentaerythritol ester, wherein the yield is 94.5%, the acid value is 22.6mgKOH/g, the softening point is 95.0 ℃, and the color and luster are measured by color comparison with Garner.
Claims (1)
1. A preparation method of rosin pentaerythritol ester is characterized by comprising the following steps: putting 100.0g of rosin, 1.5g of zinc lactate as a catalyst and 20.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in a reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 40kPa, heating to 200 ℃, and stirring for reaction for 7 hours to obtain a product, namely rosin pentaerythritol ester;
or putting 100.0g of rosin, 0.50g of zinc gluconate serving as a catalyst and 22.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in the reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 10kPa, heating to 180 ℃, and stirring for reacting for 8 hours to obtain a product, namely rosin pentaerythritol ester;
or putting 100.0g of rosin, 0.1g of catalyst ferric gluconate and 25.0g of pentaerythritol into a reaction kettle provided with a stirrer, a thermometer, an oil-water separator and a vacuum system, replacing air in the reaction system with 200kPa nitrogen for 5 times, starting the vacuum system, controlling the absolute pressure of the reaction system to be 10kPa, heating to 150 ℃, and stirring for 12 hours to obtain the product, namely the rosin pentaerythritol ester.
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