CN117143307A - Synthesis method of toughened anti-corrosion furan resin - Google Patents
Synthesis method of toughened anti-corrosion furan resin Download PDFInfo
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- CN117143307A CN117143307A CN202310771723.0A CN202310771723A CN117143307A CN 117143307 A CN117143307 A CN 117143307A CN 202310771723 A CN202310771723 A CN 202310771723A CN 117143307 A CN117143307 A CN 117143307A
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- furan resin
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- 239000007849 furan resin Substances 0.000 title claims abstract description 32
- 238000005260 corrosion Methods 0.000 title claims abstract description 22
- 238000001308 synthesis method Methods 0.000 title claims abstract description 12
- 239000000376 reactant Substances 0.000 claims abstract description 85
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 59
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 57
- 238000001816 cooling Methods 0.000 claims abstract description 47
- 238000006243 chemical reaction Methods 0.000 claims abstract description 40
- 238000003756 stirring Methods 0.000 claims abstract description 38
- 239000004202 carbamide Substances 0.000 claims abstract description 32
- 241000229722 Perilla <angiosperm> Species 0.000 claims abstract description 24
- 235000004347 Perilla Nutrition 0.000 claims abstract description 18
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 10
- 238000007599 discharging Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract 9
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 claims description 81
- 238000010438 heat treatment Methods 0.000 claims description 25
- 238000004321 preservation Methods 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 10
- 239000003377 acid catalyst Substances 0.000 claims description 9
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 7
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 6
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims 7
- 230000000694 effects Effects 0.000 abstract description 4
- 230000018044 dehydration Effects 0.000 abstract 1
- 238000006297 dehydration reaction Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 7
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229920001187 thermosetting polymer Polymers 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical group C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005058 metal casting Methods 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G16/00—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00
- C08G16/02—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes
- C08G16/04—Chemically modified polycondensates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G16/00—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00
- C08G16/02—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes
- C08G16/025—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes with heterocyclic organic compounds
- C08G16/0256—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes with heterocyclic organic compounds containing oxygen in the ring
- C08G16/0262—Furfuryl alcohol
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention discloses a synthesis method of toughened anti-corrosion furan resin, which comprises the following steps of S1: adding formaldehyde into a reaction kettle; s2: cooling the reactant in the first step to below 45 ℃; s3: adding urea; s4: negative pressure dehydration, adding a silane coupling agent, stirring uniformly, and cooling and discharging for standby reactant; s5: putting the reactant in the fourth step into a stirring tank, and putting the perilla extract into the stirring tank; s6: and (5) cooling the reactant in the step five to normal temperature to obtain a finished product. According to the invention, after the perilla extract is added into the reactant, the anti-corrosion effect of furan resin can be effectively improved, the formaldehyde release content of furan resin can be reduced, and the method is more practical and suitable for wide popularization and use.
Description
Technical Field
The invention relates to the technical field of furan resin synthesis, in particular to a synthesis method of toughened anti-corrosion furan resin.
Background
The furan resin is a resin generic term produced by taking furfuryl alcohol with furan rings and furfural as raw materials, has the advantages of water resistance, heat resistance, acid resistance, alkali resistance and the like, and is suitable for the fields of machine manufacturing, nonferrous metal casting, chemical industry and the like.
The thermosetting resin plugging material is generally formed into a high-strength plugging material through curing reaction under certain conditions by adding auxiliary agents such as a curing agent, a catalyst, an accelerator, a toughening agent and the like. The thermosetting resin plugging material has the characteristics of high compressive strength, good salt resistance and acid resistance and good aging stability, so that the thermosetting resin plugging material is widely applied. Furan resin is a common thermosetting resin, which refers to the general name of resins produced by taking furfuryl alcohol with barking rings and furfural as raw materials, and liquid furan resin can generate condensation reaction when meeting heat or acid to form a body-type structure for curing. The furan resin is synthesized by formaldehyde, furfuryl alcohol, urea, acetone or phenol and other raw materials under certain conditions.
The formaldehyde release content of the furan resin is high at a high temperature, so that the aim of environmental protection cannot be achieved, the formaldehyde can not be increased in the raw materials, and the raw materials for absorbing and adsorbing the formaldehyde can be innovated.
Disclosure of Invention
The invention aims to provide a synthesis method of toughened anti-corrosion furan resin, which solves the problems that the formaldehyde release content of furan resin is high and the aim of environmental protection cannot be achieved in the high-temperature state, so that the formaldehyde can not be increased in raw materials, and raw materials for absorbing and adsorbing formaldehyde can be innovated.
In order to achieve the above purpose, the present invention provides the following technical solutions: the synthesis method of the toughened anti-corrosion furan resin comprises the following preparation and synthesis steps:
s1: adding formaldehyde into a reaction kettle, maintaining the temperature at 80-90 ℃, adding urea and furfuryl alcohol, adjusting the PH to be 8-10, completely dissolving the furfuryl alcohol, and carrying out heat preservation reaction for 0.4-1.8h to obtain a reactant for standby;
s2: cooling the reactant in the first step to below 45 ℃, adding a proper amount of urea, adjusting the PH=4-6 by using an acid catalyst, heating to 70-80 ℃, and reacting for 0.5-1.8h to obtain the reactant;
s3: cooling the reactant in the second step to below 40 ℃, adding urea, and adjusting the PH=7-10 by using an alkaline catalyst;
s4: cooling the reactant in the third step to below 40 ℃, dehydrating under negative pressure, adding a silane coupling agent, uniformly stirring, and cooling and discharging for standby reactant;
s5: putting the reactant in the fourth step into a stirring tank, putting 20-45 g of perilla extract, heating and stirring for reaction;
s6: and (5) cooling the reactant in the step five to normal temperature to obtain a finished product.
In a preferred embodiment of the present invention, in S1, a curing agent is added to perform the curing treatment.
In a preferred embodiment of the present invention, in S2, an ethylene-vinyl acetate copolymer is added to perform a temperature-raising reaction, and a reaction heat-preserving treatment is also required.
As a preferred embodiment of the invention, the ethylene-vinyl acetate copolymer is heated to 60-85 ℃ and is subjected to thermal insulation reaction.
As a preferred embodiment of the present invention, the perilla extract is obtained by crushing the cleaned perilla plant, squeezing the crushed perilla plant, extracting the crushed perilla plant, and filtering the crushed perilla plant to obtain an extract which does not precipitate.
As a preferred embodiment of the invention, in the step one, urea and furfuryl alcohol are added, the PH=8-10 is adjusted to enable the furfuryl alcohol to be completely dissolved, the stirring motor time is 0.5h-1.3h, and the stirring speed is 900r/min.
In the fifth step, 20-45 g of perilla extract is added, heated and stirred for reaction, the heating temperature is kept between 55 ℃ and 90 ℃, and the stirring time is 10min-30 min.
As a preferred embodiment of the invention, the temperature of the reactant in the third step is raised to 80-90 ℃ and the reactant reacts for 0.3-0.6h to obtain a new reactant.
Compared with the prior art, the invention has the following beneficial effects:
according to the synthesis method of the toughened anti-corrosion furan resin, provided by the invention, the anti-corrosion effect of the furan resin can be effectively improved and the formaldehyde release content of the furan resin can be reduced by adding the perilla extract into the reactant.
Detailed Description
The invention is further described in connection with the following detailed description, in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the invention easy to understand.
Embodiment one:
the invention provides a technical scheme that: the synthesis method of the toughened anti-corrosion furan resin comprises the following preparation and synthesis steps:
s1: adding formaldehyde into a reaction kettle, maintaining the temperature at 80-90 ℃, adding urea and furfuryl alcohol, adjusting the PH to be 8-10, completely dissolving the furfuryl alcohol, and carrying out heat preservation reaction for 0.4-1.8h to obtain a reactant for standby;
s2: cooling the reactant in the first step to below 45 ℃, adding a proper amount of urea, adjusting the PH=4-6 by using an acid catalyst, heating to 70-80 ℃, and reacting for 0.5-1.8h to obtain the reactant;
s3: cooling the reactant in the second step to below 40 ℃, adding urea, and adjusting the PH=7-10 by using an alkaline catalyst;
s4: cooling the reactant in the third step to below 40 ℃, dehydrating under negative pressure, adding a silane coupling agent, uniformly stirring, and cooling and discharging for standby reactant;
s5: putting the reactant in the fourth step into a stirring tank, putting 20-45 g of perilla extract, heating and stirring for reaction;
s6: and (5) cooling the reactant in the step five to normal temperature to obtain a finished product.
Embodiment one:
the invention provides a technical scheme different from the embodiment: the synthesis method of the toughened anti-corrosion furan resin comprises the following preparation and synthesis steps:
s1: adding formaldehyde into a reaction kettle, maintaining the temperature at 85 ℃, adding urea and furfuryl alcohol, adjusting the PH to be 8.5, completely dissolving the furfuryl alcohol, and carrying out heat preservation reaction for 1.2 hours to obtain a reactant for standby;
s2: cooling the reactant in the first step to below 45 ℃, adding a proper amount of urea, adjusting the PH=4.5 by using an acid catalyst, heating to 75 ℃, and reacting for 1.3 hours to obtain the reactant;
s3: cooling the reactant in the second step to below 40 ℃, adding urea, and adjusting the PH=8 by using an alkaline catalyst;
s4: cooling the reactant in the third step to below 40 ℃, dehydrating under negative pressure, adding a silane coupling agent, uniformly stirring, and cooling and discharging for standby reactant;
s5: putting the reactant in the fourth step into a stirring tank, putting 30 g of perilla extract, heating and stirring for reaction;
s6: and (5) cooling the reactant in the step five to normal temperature to obtain a finished product.
In this embodiment, in S1, a curing agent is required to be added for curing treatment; s2, adding an ethylene-vinyl acetate copolymer for heating reaction, and carrying out reaction heat preservation treatment; heating the ethylene-vinyl acetate copolymer to 60-85 ℃, and carrying out heat preservation reaction; the perilla extract is obtained by crushing, squeezing, extracting and filtering the cleaned perilla plant, and forms an extract which does not precipitate.
Embodiment two:
the invention provides a technical scheme different from the embodiment: the synthesis method of the toughened anti-corrosion furan resin comprises the following preparation and synthesis steps:
s1: adding formaldehyde into a reaction kettle, maintaining the temperature at 85 ℃, adding urea and furfuryl alcohol, adjusting the PH to be 8.5, completely dissolving the furfuryl alcohol, and carrying out heat preservation reaction for 1.2 hours to obtain a reactant for standby;
s2: cooling the reactant in the first step to below 45 ℃, adding a proper amount of urea, adjusting the PH=4.5 by using an acid catalyst, heating to 75 ℃, and reacting for 1.3 hours to obtain the reactant;
s3: cooling the reactant in the second step to below 40 ℃, adding urea, and adjusting the PH=8 by using an alkaline catalyst;
s4: cooling the reactant in the third step to below 40 ℃, dehydrating under negative pressure, adding a silane coupling agent, uniformly stirring, and cooling and discharging for standby reactant;
s5: putting the reactant in the fourth step into a stirring tank, putting 35 g of perilla extract, heating and stirring for reaction;
s6: and (5) cooling the reactant in the step five to normal temperature to obtain a finished product.
In the embodiment, in the first step, urea and furfuryl alcohol are added, the PH=8-10 is regulated, the furfuryl alcohol is completely dissolved, the time of a stirring motor is 0.5h-1.3h, and the stirring speed is 900r/min; step five, adding 20-45 g of perilla extract, heating and stirring for reaction, wherein the heating temperature is kept at 55-90 ℃, and the stirring time is 10-30 min; and step three, heating the reactant to 80-90 ℃ and reacting for 0.3-0.6h to obtain a new reactant.
Comparative example 1:
the invention provides a technical scheme different from the embodiment: the synthesis method of the toughened anti-corrosion furan resin comprises the following preparation and synthesis steps:
s1: adding formaldehyde into a reaction kettle, maintaining the temperature at 85 ℃, adding urea and furfuryl alcohol, adjusting the PH to be 8.5, completely dissolving the furfuryl alcohol, and carrying out heat preservation reaction for 1.2 hours to obtain a reactant for standby;
s2: cooling the reactant in the first step to below 45 ℃, adding a proper amount of urea, adjusting the PH=4.5 by using an acid catalyst, heating to 75 ℃, and reacting for 1.3 hours to obtain the reactant;
s3: cooling the reactant in the second step to below 40 ℃, adding urea, and adjusting the PH=8 by using an alkaline catalyst;
s4: and (3) cooling the reactant in the step (III) to below 40 ℃, dehydrating under negative pressure, adding a silane coupling agent, uniformly stirring, and cooling and discharging for standby reactant to obtain a finished product.
Comparative example 2:
s1: adding formaldehyde into a reaction kettle, maintaining the temperature at 85 ℃, adding urea and furfuryl alcohol, adjusting the PH to be 8.5, completely dissolving the furfuryl alcohol, and carrying out heat preservation reaction for 1.2 hours to obtain a reactant for standby;
s2: cooling the reactant in the first step to below 45 ℃, adding a proper amount of urea, adjusting the PH=4.5 by using an acid catalyst, heating to 75 ℃, and reacting for 1.3 hours to obtain the reactant;
s3: cooling the reactant in the second step to below 40 ℃, adding urea, and adjusting the PH=8 by using an alkaline catalyst;
s4: cooling the reactant in the third step to below 40 ℃, dehydrating under negative pressure, adding a silane coupling agent, uniformly stirring, and cooling and discharging for standby reactant;
s5: putting the reactant in the fourth step into a stirring tank, putting 10 g of perilla extract, heating and stirring for reaction;
s6: and (5) cooling the reactant in the step five to normal temperature to obtain a finished product.
Comparative example 3:
s1: adding formaldehyde into a reaction kettle, maintaining the temperature at 85 ℃, adding urea and furfuryl alcohol, adjusting the PH to be 8.5, completely dissolving the furfuryl alcohol, and carrying out heat preservation reaction for 1.2 hours to obtain a reactant for standby;
s2: cooling the reactant in the first step to below 45 ℃, adding a proper amount of urea, adjusting the PH=4.5 by using an acid catalyst, heating to 75 ℃, and reacting for 1.3 hours to obtain the reactant;
s3: cooling the reactant in the second step to below 40 ℃, adding urea, and adjusting the PH=8 by using an alkaline catalyst;
s4: cooling the reactant in the third step to below 40 ℃, dehydrating under negative pressure, adding a silane coupling agent, uniformly stirring, and cooling and discharging for standby reactant;
s5: putting the reactant in the fourth step into a stirring tank, putting 48 g of perilla extract, heating and stirring for reaction;
s6: and (5) cooling the reactant in the step five to normal temperature to obtain a finished product.
The following table shows the variation in the reactants in each example;
from the table, it can be known that in the scheme, after the perilla extract is added into the reactant, the anti-corrosion effect of the furan resin can be effectively improved, and the formaldehyde release content of the furan resin can be effectively reduced.
Working principle:
s1: adding formaldehyde into a reaction kettle, maintaining the temperature at 85 ℃, adding urea and furfuryl alcohol, adjusting the PH to be 8.5, completely dissolving the furfuryl alcohol, and carrying out heat preservation reaction for 1.2 hours to obtain a reactant for standby;
s2: cooling the reactant in the first step to below 45 ℃, adding a proper amount of urea, adjusting the PH=4.5 by using an acid catalyst, heating to 75 ℃, and reacting for 1.3 hours to obtain the reactant;
s3: cooling the reactant in the second step to below 40 ℃, adding urea, and adjusting the PH=8 by using an alkaline catalyst;
s4: cooling the reactant in the third step to below 40 ℃, dehydrating under negative pressure, adding a silane coupling agent, uniformly stirring, and cooling and discharging for standby reactant;
s5: putting the reactant in the fourth step into a stirring tank, putting 30 g of perilla extract, heating and stirring for reaction;
s6: and (5) cooling the reactant in the step five to normal temperature to obtain a finished product.
Claims (8)
1. The synthesis method of the toughened anti-corrosion furan resin is characterized by comprising the following preparation and synthesis steps:
s1: adding formaldehyde into a reaction kettle, maintaining the temperature at 80-90 ℃, adding urea and furfuryl alcohol, adjusting the PH to be 8-10, completely dissolving the furfuryl alcohol, and carrying out heat preservation reaction for 0.4-1.8h to obtain a reactant for standby;
s2: cooling the reactant in the first step to below 45 ℃, adding a proper amount of urea, adjusting the PH=4-6 by using an acid catalyst, heating to 70-80 ℃, and reacting for 0.5-1.8 hours to obtain the reactant;
s3: cooling the reactant in the second step to below 40 ℃, adding urea, and adjusting the PH=7-10 by using an alkaline catalyst;
s4: cooling the reactant in the third step to below 40 ℃, dehydrating under negative pressure, adding a silane coupling agent, uniformly stirring, and cooling and discharging for standby reactant;
s5: putting the reactant in the fourth step into a stirring tank, putting 20-45 g of perilla extract, heating and stirring for reaction;
s6: and (5) cooling the reactant in the step five to normal temperature to obtain a finished product.
2. The method for synthesizing the toughened anti-corrosion furan resin according to claim 1, which is characterized in that: in the step S1, a curing agent is required to be added for curing treatment.
3. The method for synthesizing the toughened anti-corrosion furan resin according to claim 2, which is characterized in that: and in the step S2, an ethylene-vinyl acetate copolymer is put in for heating reaction, and the reaction is carried out for heat preservation.
4. The method for synthesizing the toughened anti-corrosion furan resin according to claim 3, wherein the method comprises the following steps: the ethylene-vinyl acetate copolymer is heated to 60-85 ℃ and reacts at a constant temperature.
5. The method for synthesizing the toughened anti-corrosion furan resin according to claim 1, which is characterized in that: the perilla extract is obtained by crushing, squeezing, extracting and filtering the cleaned perilla plants, and forms an extract which cannot be precipitated.
6. The method for synthesizing the toughened anti-corrosion furan resin according to claim 1, which is characterized in that: and in the first step, urea and furfuryl alcohol are added, the PH=8-10 is regulated, the furfuryl alcohol is completely dissolved, the time of a stirring motor is 0.5h-1.3h, and the stirring speed is 900r/min.
7. The method for synthesizing the toughened anti-corrosion furan resin according to claim 1, which is characterized in that: in the fifth step, 20-45 g of perilla extract is added, heated and stirred for reaction, the heating temperature is kept at 55-90 ℃, and the stirring time is 10-30 min.
8. The method for synthesizing the toughened anti-corrosion furan resin according to claim 1, which is characterized in that: and in the third step, the temperature of the reactant is raised to 80-90 ℃ and the reaction is carried out for 0.3-0.6h to obtain a new reactant.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310771723.0A CN117143307A (en) | 2023-06-28 | 2023-06-28 | Synthesis method of toughened anti-corrosion furan resin |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310771723.0A CN117143307A (en) | 2023-06-28 | 2023-06-28 | Synthesis method of toughened anti-corrosion furan resin |
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