CN111087563A - Modified phenolic resin, preparation method and refractory material containing modified phenolic resin - Google Patents
Modified phenolic resin, preparation method and refractory material containing modified phenolic resin Download PDFInfo
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- 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
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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- C04B2235/77—Density
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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- Health & Medical Sciences (AREA)
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- Compositions Of Oxide Ceramics (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention discloses a preparation method of modified phenolic resin for refractory materials, which comprises the following steps: adding papermaking waste, phenol and an acid catalyst into a reaction kettle for blending; after the temperature is raised, aldehyde is dropwise added into the reaction kettle, and the reaction is fully carried out after the addition is finished; vacuum dehydration is carried out, the vacuum is released when the temperature is 100-130 ℃, and the reaction is continued; and performing reduced pressure dehydration again to obtain the phenolic resin for the refractory material. The invention further provides a refractory material, which comprises the following components in parts by weight: 40-75 parts of magnesia-calcium sand; 20-50 parts of aluminum oxide; 7-18 parts of carbon and 3-9 parts of modified phenolic resin. The modified phenolic resin of the invention adopts papermaking waste to carry out chemical modification on the phenolic resin, thereby effectively improving the heat resistance of the resin, simultaneously improving the carbon residue rate and the bonding strength of the resin, and the high-temperature strength of the prepared refractory material is higher than that of the conventional phenolic resin.
Description
Technical Field
The invention relates to the technical field of phenolic resin application, in particular to modified phenolic resin, a preparation method thereof and a refractory material containing the modified phenolic resin.
Background
The phenolic resin is synthetic resin which is industrially produced at the earliest time in the world, has excellent flame retardance, electrical property and insulating property, and has wide application in the fields of composite materials, coatings, foam materials, adhesives, printing ink and the like. In addition, phenolic resins are used in very large amounts in the context of refractory binders, in particular with regard to their high carbon residue and temperature resistance.
As a binder of a refractory material, resin is required to have high temperature resistance and thermal stability and have high carbon residue rate after carbonization so as to ensure the strength of the material at high temperature. However, the carbon residue of phenolic resin commonly used at present is about 60%, and the heat resistance is still to be improved.
Disclosure of Invention
The invention aims to provide a modified phenolic resin, a preparation method thereof and a refractory material containing the modified phenolic resin, so as to solve the defects in the background art.
The invention is realized by the following technical scheme:
a preparation method of modified phenolic resin comprises the following steps:
step one, adding papermaking waste, phenol and an acid catalyst into a reaction kettle for blending;
step two, dripping aldehyde into the reaction kettle after heating, and fully reacting after adding;
step three, vacuum dehydration is carried out, the vacuum is released when the temperature is 100-;
and step four, performing reduced pressure dehydration again to obtain the phenolic resin for the refractory material.
The weight parts of the components are as follows: 30-50 parts of papermaking waste, 50-70 parts of phenol, 1-8 parts of acid catalyst and 45-55 parts of aldehyde.
The papermaking waste is any one of dilute acid hydrolysate, dilute black liquor, concentrated acid hydrolysate, hydrolyzed lignin, sulfonate, enzymolyzed lignin or derivatives thereof in the wood hydrolysis industry and papermaking industry waste.
The phenol is selected from at least one of phenol, cresol, m-cresol and bisphenol A, and is preferably phenol.
The acidic catalyst is selected from at least one of oxalic acid, hydrochloric acid, sulfuric acid, phosphoric acid, phosphonic acid, benzenesulfonic acid, acetic acid, carbonic acid, ammonium chloride and p-toluenesulfonic acid, and preferably at least one of oxalic acid, hydrochloric acid and phosphoric acid.
The aldehyde is selected from at least one of formaldehyde, paraformaldehyde, acetaldehyde, propionaldehyde and butyraldehyde, and is preferably formaldehyde.
Preferably, in the second step, formaldehyde is added dropwise after the temperature is raised to 60-85 ℃, and the temperature is kept at 90-120 ℃ after the addition is finished, so that the reaction lasts for 2-4 hours.
Preferably, in the third step, vacuum dehydration is carried out under the reduced pressure of 0.09MPa, and the reaction is continued for 1 to 3 hours after the vacuum is relieved.
The invention provides the modified phenolic resin prepared by the method, wherein the free phenol is less than or equal to 0.5 percent, and the free aldehyde is less than or equal to 0.3 percent.
The invention further provides a refractory material, which comprises the following components in parts by weight: 40-75 parts of magnesia-calcium sand, 20-50 parts of alumina, 7-18 parts of carbon and 3-9 parts of modified phenolic resin.
Preferably, the carbon is graphite or carbon black.
The invention further provides a preparation method of the refractory material, which comprises the following steps: mixing the magnesia-calcium sand and the alumina to obtain a premix, adding the premix, the modified phenolic resin and the carbon into a mixer to mix to obtain a mixed material, putting the mixed material into an isostatic pressing machine mould, carrying out pressure molding, putting the obtained molded product into a kiln channel to be burnt to the temperature of 300 ℃ and 400 ℃, polishing the product after the product is taken out of the kiln, and coating an antioxidant material to obtain the refractory material.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the phenolic resin is modified by using papermaking waste, so that the heat resistance of the resin can be effectively improved, and the carbon residue rate and the bonding strength of the resin are improved;
2. the invention uses the papermaking waste to make a certain contribution to relieving the pressure of the papermaking environment;
3. the invention achieves the same performance, and simultaneously has less formaldehyde consumption and larger molecular structure density.
Detailed Description
The invention is illustrated below by means of specific examples, without being restricted thereto. Unless otherwise specified, each raw material is a commercially available product. Paper waste is provided by the new Jinming material company, Inc.
Example 1
1) Adding 30g of papermaking waste, 70g of phenol and 2g of oxalic acid catalyst into a reaction kettle;
2) heating to 60 ℃, dropwise adding 50g of formaldehyde into the reaction kettle, and keeping the temperature at 90 ℃ for 3h after the addition is finished;
3) vacuum dehydrating under reduced pressure of 0.09MPa, relieving vacuum at 100 deg.C, stirring, and reacting for 3 hr;
4) and carrying out decompression dehydration again to obtain the modified phenolic resin for the refractory material.
5) The obtained phenolic resin is used to prepare a refractory material.
The preparation method of the refractory material comprises the following steps:
40 parts of magnesia-calcium sand and 20 parts of alumina are mixed to obtain a premix, the premix is added into a mixer and is mixed with 3 parts of the papermaking waste modified phenolic resin obtained in the embodiment 1 for 5min, 7 parts of carbon is added and is mixed for 30min to obtain a mixed material, the mixed material is placed into an isostatic pressing machine die for pressure forming, the obtained formed product is placed into a kiln channel to be burnt to 300 ℃, the product taken out of the kiln is polished and coated with an antioxidant material to obtain the refractory material.
Example 2
1) Adding 40g of papermaking waste, 60g of phenol and 4g of hydrochloric acid catalyst into a reaction kettle;
2) heating to 70 ℃, dropwise adding 50g of formaldehyde into the reaction kettle, and keeping the temperature at 100 ℃ for 4h after the addition is finished;
3) vacuum dehydrating under reduced pressure of 0.09MPa, relieving vacuum at 110 deg.C, stirring, and reacting for 2 hr;
4) and carrying out decompression dehydration again to obtain the phenolic resin for the refractory material.
5) The obtained phenolic resin is used to prepare a refractory material.
The preparation method of the refractory material comprises the following steps:
50 parts of magnesia-calcium sand and 30 parts of alumina are mixed to obtain a premix, the premix and 6 parts of the paper-making waste modified phenolic resin obtained in the embodiment 2 are added into a mixer to be mixed for 5min, 15 parts of carbon is added to be mixed for 30min to obtain a mixed material, the mixed material is placed into an isostatic pressing machine mould to be pressed and formed, the formed product is placed into a kiln channel to be burnt to 300 ℃, the product taken out of the kiln is polished, and an antioxidant material is coated to obtain the refractory material.
Example 3
1) Adding 50g of papermaking waste, 50g of phenol and 7g of phosphoric acid catalyst into a reaction kettle;
2) heating to 85 ℃, dropwise adding 50g of formaldehyde into the reaction kettle, and keeping the temperature at 120 ℃ for 2h after the addition is finished;
3) vacuum dehydrating under reduced pressure of 0.09MPa, relieving vacuum at 130 deg.C, stirring, and reacting for 1 h;
4) and carrying out decompression dehydration again to obtain the phenolic resin for the refractory material.
5) The obtained phenolic resin is used to prepare a refractory material.
The preparation method of the refractory material comprises the following steps:
75 parts of magnesia-calcium sand and 50 parts of alumina are mixed to obtain a premix, the premix and 9 parts of the paper-making waste modified phenolic resin obtained in the embodiment 3 are added into a mixer to be mixed for 5min, 18 parts of carbon is added to be mixed for 30min to obtain a mixed material, the mixed material is placed into an isostatic pressing machine die to be pressed and molded, the molded product is placed into a kiln channel to be burnt to 300 ℃, the product taken out of the kiln is polished, and an antioxidant material is coated to obtain the refractory material.
Comparative example 1
1) Adding 70g of phenol and 2g of phosphoric acid catalyst into a reaction kettle;
2) heating to 60 ℃, dropwise adding 35g of formaldehyde into the reaction kettle, and keeping the temperature at 90 ℃ for 3h after the addition is finished;
3) vacuum dehydrating under reduced pressure of 0.09MPa, relieving vacuum at 100 deg.C, stirring, and reacting for 3 hr;
4) and carrying out decompression dehydration again to obtain the phenolic resin for the refractory material.
5) The obtained phenolic resin is used to prepare a refractory material.
The preparation method of the refractory material comprises the following steps:
40 parts of magnesia-calcium sand and 20 parts of alumina are mixed to obtain a premix, the premix and 3 parts of the phenolic resin obtained in the comparative example 1 are added into a mixer to be mixed for 5min, 7 parts of carbon is added to be mixed for 30min to obtain a mixed material, the mixed material is placed into an isostatic pressing machine die to be pressed and molded, the molded product is placed into a kiln channel to be burnt to 300 ℃, and the product after being taken out of the kiln is polished and coated with an antioxidant material to obtain the refractory material.
Comparative example 2
1) Adding 60g of phenol and 1.7g of p-toluenesulfonic acid catalyst into a reaction kettle;
2) heating to 70 ℃, dropwise adding 30g of formaldehyde into the reaction kettle, and keeping the temperature at 100 ℃ for 4h after the addition is finished;
3) vacuum dehydrating under reduced pressure of 0.09MPa, relieving vacuum at 110 deg.C, stirring, and reacting for 2 hr;
4) and carrying out decompression dehydration again to obtain the phenolic resin for the refractory material.
5) The obtained phenolic resin is used to prepare a refractory material.
The preparation method of the refractory material comprises the following steps:
50 parts of magnesia-calcium sand and 30 parts of alumina are mixed to obtain a premix, the premix and 6 parts of the phenolic resin obtained in the comparative example 2 are added into a mixer to be mixed for 5min, 15 parts of carbon is added to be mixed for 30min to obtain a mixed material, the mixed material is placed into an isostatic pressing machine die to be pressed and molded, the molded product is placed into a kiln channel to be burnt to 300 ℃, and the product taken out of the kiln is polished and coated with an antioxidant material to obtain the refractory material.
Comparative example 3
1) Adding 50g of phenol and 1.5g of benzenesulfonic acid catalyst into a reaction kettle;
2) heating to 85 ℃, dropwise adding 25g of formaldehyde into the reaction kettle, and keeping the temperature at 120 ℃ for 2h after the addition is finished;
3) vacuum dehydrating under reduced pressure of 0.09MPa, relieving vacuum at 130 deg.C, stirring, and reacting for 1 h;
4) and carrying out decompression dehydration again to obtain the phenolic resin for the refractory material.
5) The obtained phenolic resin is used to prepare a refractory material.
The preparation method of the refractory material comprises the following steps:
75 parts of magnesia-calcium sand and 50 parts of alumina are mixed to obtain a premix, the premix and 9 parts of the phenolic resin obtained in the comparative example 3 are added into a mixer to be mixed for 5min, 18 parts of carbon is added to be mixed for 30min to obtain a mixed material, the mixed material is placed into an isostatic pressing machine die to be pressed and molded, the molded product is placed into a kiln channel to be burnt to 300 ℃, and the product taken out of the kiln is polished and coated with an antioxidant material to obtain the refractory material.
The physical properties and special properties of the refractory material are measured by adopting the methods of GB/T4513-2017, GB/T5072-2008, GB/T3002-2004 and other standards. The specific test results are shown in Table 1. Wherein the test temperature of the high-temperature rupture strength is 1400 ℃, and the heat preservation time is 30 min.
TABLE 1 index of performance of refractory
As can be seen from the detection data of the examples and the comparative examples, the experimental data of the invention are obviously superior to that of the common phenolic resin, and particularly the high-temperature rupture strength is higher than that of the comparative example 53.85%. The modified phenolic resin for the refractory material disclosed by the invention is prepared by chemically modifying phenolic resin by adopting papermaking waste, so that the heat resistance of the resin is effectively improved, and the carbon residue rate and the bonding strength of the resin are improved.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The preparation method of the modified phenolic resin is characterized by comprising the following steps:
step one, adding papermaking waste, phenol and an acid catalyst into a reaction kettle for blending;
step two, dripping aldehyde into the reaction kettle after heating, and fully reacting after adding;
step three, vacuum dehydration is carried out, the vacuum is released when the temperature is 100-;
and step four, performing reduced pressure dehydration again to obtain the phenolic resin for the refractory material.
2. The method of claim 1, wherein the weight parts of each component are as follows: 30-50 parts of papermaking waste, 50-70 parts of phenol, 1-8 parts of acid catalyst and 45-55 parts of aldehyde.
3. The method according to claim 1, wherein the paper-making waste is any one of dilute acid hydrolysate, dilute black liquor, concentrated acid hydrolysate, hydrolyzed lignin, sulfonate, enzymatic hydrolyzed lignin or derivatives thereof in wood hydrolysis industry and paper-making industry waste.
4. The method of claim 1, wherein the phenol is phenol and the aldehyde is formaldehyde.
5. The method of claim 1, wherein the acidic catalyst is selected from at least one of oxalic acid, hydrochloric acid, and phosphoric acid.
6. The method of claim 1, wherein in the second step, formaldehyde is added dropwise after the temperature is raised to 60-85 ℃, and the temperature is kept at 90-120 ℃ after the addition is finished, and the reaction is carried out for 2-4 hours.
7. The method of claim 1, wherein in the third step, vacuum dehydration is performed under reduced pressure of 0.09MPa, and the reaction is continued for 1-3h after the vacuum is released.
8. The modified phenolic resin produced by the method of any one of claims 1 to 7, wherein the free phenol is 0.5% or less and the free aldehyde is 0.3% or less.
9. The refractory material is characterized by comprising the following components in parts by weight: 40-75 parts of magnesia-calcium sand, 20-50 parts of alumina, 7-18 parts of carbon and 3-9 parts of the modified phenolic resin of claim 8.
10. A preparation method of a refractory material comprises the following steps: mixing the magnesia-calcium sand and the alumina to obtain a premix, adding the premix, the modified phenolic resin as claimed in claim 8 and carbon into a mixer to mix to obtain a mixed material, putting the mixed material into an isostatic pressing machine die, carrying out pressure molding, putting the obtained molded product into a kiln channel to be fired to 300-400 ℃, polishing the product after the product is taken out of the kiln, and coating an antioxidant material to obtain the refractory material.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU6071086A (en) * | 1985-07-31 | 1987-02-05 | Borden Chemical, Inc. | Process for preparing phenolic resin binders for foundry and refractory uses |
| CN102127197A (en) * | 2010-12-01 | 2011-07-20 | 山东圣泉化工股份有限公司 | Preparation method for phenolic resin for magnesia-carbon brick |
| CN109679547A (en) * | 2018-12-20 | 2019-04-26 | 上海昶法新材料有限公司 | A kind of preparation method of modified phenolic resin adhesive and products thereof |
| CN110317308A (en) * | 2019-07-16 | 2019-10-11 | 沙县宏盛塑料有限公司 | A kind of preparation method and refractory material of phenolic resin for refractory material |
| CN110564346A (en) * | 2019-09-20 | 2019-12-13 | 上海昶法新材料有限公司 | Modified phenolic glue and preparation method thereof |
-
2019
- 2019-12-25 CN CN201911358573.0A patent/CN111087563A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU6071086A (en) * | 1985-07-31 | 1987-02-05 | Borden Chemical, Inc. | Process for preparing phenolic resin binders for foundry and refractory uses |
| CN102127197A (en) * | 2010-12-01 | 2011-07-20 | 山东圣泉化工股份有限公司 | Preparation method for phenolic resin for magnesia-carbon brick |
| CN109679547A (en) * | 2018-12-20 | 2019-04-26 | 上海昶法新材料有限公司 | A kind of preparation method of modified phenolic resin adhesive and products thereof |
| CN110317308A (en) * | 2019-07-16 | 2019-10-11 | 沙县宏盛塑料有限公司 | A kind of preparation method and refractory material of phenolic resin for refractory material |
| CN110564346A (en) * | 2019-09-20 | 2019-12-13 | 上海昶法新材料有限公司 | Modified phenolic glue and preparation method thereof |
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